CN112111047A - High-peel hydrolysis-resistant polyurethane resin and preparation method thereof - Google Patents
High-peel hydrolysis-resistant polyurethane resin and preparation method thereof Download PDFInfo
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- C08G18/40—High-molecular-weight compounds
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
- C08G18/4236—Polycondensates having carboxylic or carbonic ester groups in the main chain containing only aliphatic groups
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- C08G18/48—Polyethers
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Abstract
The invention discloses a high-peel hydrolysis-resistant polyurethane resin which is prepared from the following raw materials in parts by weight: poly (1, 6-hexanediol adipate) glycol: 15-25 parts of polytetrahydrofuran diol PTMEG-3000: 20-27 parts of polyethylene glycol: 50-70 parts of trimethylolpropane: 5.5-8.5 parts of 4,4' -diphenylmethane diisocyanate: 10-12 parts of xylylene diisocyanate: 5-6.5 parts of organic bismuth catalyst: 0.2-0.35 parts of isophorone diamine: 3.5-4.5 parts of KH-560: 2.5-3.5 parts of an organic silicon anti-sticking agent: 0.5 to 0.8 portion. The high-peel hydrolysis-resistant polyurethane resin disclosed by the invention is high in peel strength, good in hydrolysis resistance, high in peel strength and good in hydrolysis resistance; the high-peel hydrolysis-resistant polyurethane resin can be directly coated on a textile fabric or a non-woven fabric, so that the high-peel hydrolysis-resistant polyurethane resin has high peel and good hydrolysis resistance after film formation, and a coated textile fabric or non-woven fabric finished product also has high peel and good hydrolysis resistance.
Description
Technical Field
The invention relates to the technical field of polyurethane and production equipment thereof, and particularly relates to a high-peel hydrolysis-resistant polyurethane resin and a preparation method thereof.
Background
Polyurethane is named polyurethane, which is a high molecular compound, and can be made into polyurethane plastics (mainly foamed plastics), polyurethane fibers (China called spandex), polyurethane rubber and elastomers.
The main raw materials of polyurethane comprise diphenylmethane diisocyanate (MDI), Toluene Diisocyanate (TDI) and polypropylene glycol (PPG), and are internationalized commodities at present. The production techniques and equipment for these feedstocks are complex.
The polyurethane resin is generally formed by reacting polyisocyanates, polyols and the like containing active hydrogen atoms and groups, the reaction between the polyisocyanates and the polyols is a reaction between solutions, and the reaction degree is greatly influenced by the uniform stirring in a reaction kettle; in the existing industrial reaction kettle, a stirring device is generally arranged in the actual production, but vortex can be generated in the stirring process, so that the mixing directions of reactants are the same, the mixing degree of the reactants is insufficient, and the reaction speed is slow; the invention with the application number of CN209680089U discloses a polyurethane stirring reaction kettle, which comprises a kettle body, a feeding hole, a discharging hole and supporting legs, wherein a heat-insulating jacket is arranged on the periphery of the kettle body, a cavity is formed in the kettle body, a stirring mechanism is arranged at the top of the kettle body, and the stirring mechanism comprises a stirring motor and a stirring shaft connected with the stirring motor; the polyurethane reaction kettle provided by the invention has the advantages of good material mixing uniformity, difficulty in material accumulation at the kettle bottom, high mixing efficiency, difficulty in wall adhesion and the like, and a stirring device of the polyurethane reaction kettle has certain defects.
Need carry out the material loading to the raw materials at the in-process of polyurethane production, current publication number CN209934543U discloses a loading attachment that waterborne polyurethane lacquer production used, the device discharges the raw materials into the agitator through the suction pump and realizes the material loading, but this kind of loading attachment can not adjust the height of loading attachment according to the height of different agitators, and polyurethane's heat resistance is relatively poor, when raw materials material loading, do not carry out cooling treatment to the raw materials, because the temperature can influence the chemical property of raw materials, if do not control the temperature of raw materials, can influence production quality.
The stirring mixer and the cyclone reactor in the polyurethane resin production device disclosed in publication No. CN205953901U are both conventional components, and are divided into two processing steps, so that the occupied space is large, and the mixing and reaction efficiency is difficult to improve.
Chinese patent application No. CN201720241412.3 discloses a polyurethane heating device, which includes a temperature controller, an oven, a water bath, a mold temperature controller, and a circulation oil path, wherein the mold temperature controller is connected to the circulation oil path, the oven is provided with an opening, the circulation oil path includes a first circulation oil path and a second circulation oil path, a fan is provided at the opening, a first solenoid valve is provided in front of the opening of the first circulation oil path, a second solenoid valve is provided in front of an inlet of the water bath of the second circulation oil path, but the temperature in the structure is difficult to control. The current heating reaction device for polyurethane production has the following problems: 1. the existing heating reaction device for producing polyurethane can only heat in a single mode, so that the heating rate and stability can not meet the reaction requirement; 2. the polyurethane raw material in the container of the existing heating reaction device for producing polyurethane has low heat conduction efficiency, and the production quality is poor due to uneven heating.
When the nitrogen charging device is used for producing the polyurethane material, for example, the patent application number CN201720950094.8 discloses a nitrogen charging device of a reaction kettle for producing the polyurethane material, which comprises an upper nitrogen connecting valve body and a lower nitrogen charging valve body, wherein the upper nitrogen connecting valve body is connected with the lower nitrogen charging valve body through a corresponding tongue and groove, a nitrogen connecting end orifice is arranged above the upper nitrogen connecting valve body, a port tightening ring is arranged at the outer side of the nitrogen connecting end orifice, a sealing ring is sleeved at the lower side of the port tightening ring and the nitrogen connecting end orifice, the other side end of the upper nitrogen connecting valve body is provided with a pressure supplementing interface, a rotating nut is arranged at one side end of the lower nitrogen charging valve body and is connected with the lower nitrogen charging valve body through a semi-ring clamp, an air adjusting valve rod is arranged at the inner side of the rotating nut, a pressure gauge is arranged at the lower end of the lower nitrogen charging valve body and is used for measuring the pressure of nitrogen, and is connected with the lower nitrogen charging valve body through a J-shaped, the other side end of the nitrogen charging lower valve body is set to be a nitrogen charging port, and a lock lantern ring is installed on the outer side of the nitrogen charging port, so that people can conveniently use the nitrogen charging lower valve body. However, the existing nitrogen charging device has the following problems: 1. when in use, the fixing is inconvenient, so that the normal use is influenced due to shaking when in use; 2. when the nitrogen bottle is used, the nitrogen bottle can be continuously used only by replacing the stopping device when the nitrogen amount of the nitrogen bottle is insufficient.
During the production process of polyurethane, a high-viscosity pump is often needed to be used for matching, such as the following application numbers: CN102072130A provides a water pump apparatus, which includes a base, at least two horizontal water pumps mounted on the base, and a water inlet and outlet pipeline, where the water inlet pipeline includes at least two water inlet assemblies respectively connected to water inlets of the at least two horizontal water pumps, and a water inlet header pipe communicated with the water inlet assemblies; the water outlet pipeline comprises at least two water outlet components respectively connected to the water outlets of at least two horizontal water pumps and a water outlet main pipe communicated with the water outlet components, and the water inlet main pipe and the water outlet main pipe are respectively supported on the base through a support; the base comprises a water pump base and at least one bracket base, at least two horizontal water pumps are fixedly arranged on the water pump base, and the bracket is arranged on the bracket base; the support base is connected on the water pump base with adjustable for water pump base extension length. When the water pump base is installed in a water supply network, the water pump base can adapt to the specific space condition by adjusting the extension length of the bracket base relative to the water pump base, the base does not need to be integrally replaced, the installation efficiency is greatly improved, and the cost is reduced. However, the existing high-viscosity pump has the following problems: 1. the existing high-viscosity pump is too complex when being disassembled and assembled integrally, so that the existing high-viscosity pump is inconvenient to transport and fast overhaul, and the integral use efficiency is reduced; 2. the existing high-viscosity pump has low overall corrosion resistance, wear resistance and high-temperature resistance, so that the existing high-viscosity pump is easy to damage and the overall service life is shortened.
Further, the polyurethane resin and the production apparatus thereof have the following problems:
1. the peel strength is low, and the bonding fastness of the polyurethane resin and the base cloth is not enough; the hydrolysis resistance is poor, and the surface is stained with alkaline substances, so that the peel strength is easily greatly lost, even no peel strength exists;
2. the production of polyurethane resin lacks medium and small continuous production equipment, and cannot well combine mixing, feeding, prepolymerization, polymerization, discharging and storage, so that complete continuous polyurethane production equipment cannot be formed;
3. the links of mixing, feeding, prepolymerization, polymerization, discharging, storage and the like of the polyurethane production equipment also have the defects, cannot well meet the requirements of polyurethane production, and cannot ensure the quality of the produced polyurethane.
Based on the situation, the invention provides a high-peeling hydrolysis-resistant polyurethane resin and a preparation method thereof, and the problems can be effectively solved.
Disclosure of Invention
The invention aims to provide a high-peeling hydrolysis-resistant polyurethane resin and a preparation method thereof. The high-stripping hydrolysis-resistant polyurethane resin is prepared by selecting raw materials, optimizing the content of each raw material, selecting 1, 6-hexanediol adipate, polytetrahydrofuran diol PTMEG-3000, polyethylene glycol, trimethylolpropane, 4' -diphenylmethane diisocyanate, xylylene diisocyanate, an organic bismuth catalyst, isophorone diamine, KH-560 and an organic silicon anti-sticking agent in a proper proportion, and distributing the advantages of each raw material, wherein the raw materials are matched with each other and are mutually promoted, and the high-stripping hydrolysis-resistant polyurethane resin obtained by polymerization has high stripping strength, good hydrolysis resistance and high stripping and hydrolysis resistance; the high-peel hydrolysis-resistant polyurethane resin can be directly coated on a textile fabric or a non-woven fabric, so that the high-peel hydrolysis-resistant polyurethane resin has high peel and good hydrolysis resistance after film formation, and a coated textile fabric or non-woven fabric finished product also has high peel and good hydrolysis resistance.
The invention is realized by the following technical scheme:
the high-peel hydrolysis-resistant polyurethane resin is prepared from the following raw materials in parts by weight: poly (1, 6-hexanediol adipate) glycol: 15-25 parts of polytetrahydrofuran diol PTMEG-3000: 20-27 parts of polyethylene glycol: 50-70 parts of trimethylolpropane: 5.5-8.5 parts of 4,4' -diphenylmethane diisocyanate: 10-12 parts of xylylene diisocyanate: 5-6.5 parts of organic bismuth catalyst: 0.2-0.35 parts of isophorone diamine: 3.5-4.5 parts of KH-560: 2.5-3.5 parts of an organic silicon anti-sticking agent: 0.5-0.8 part; the molecular weight of the poly adipic acid 1, 6-hexanediol glycol ester is 1500-2000; the molecular weight of the polyethylene glycol is 2000-2500; the mixture of the organosilicon antisticking agent AC-1800K and the antisticking agent FY-5080K is prepared from the following components in a mass ratio of 1: 0.75 to 0.88.
The invention also provides a preparation method of the high-peel hydrolysis-resistant polyurethane resin, which adopts polyurethane production equipment to carry out continuous production preparation and comprises the following steps:
1) weighing the raw materials of the aliphatic non-yellowing polyurethane resin according to the parts by weight;
2) putting poly adipic acid 1, 6-hexanediol glycol, polytetrahydrofuran diol PTMEG-3000, polyethylene glycol, trimethylolpropane, 1/2 4,4' -diphenylmethane diisocyanate and 1/2 xylylene diisocyanate into a mixing and stirring kettle, and uniformly mixing to obtain a mixture;
3) conveying the mixture into a prepolymer tubular reactor by using a feeding device, performing prepolymerization, controlling the temperature in the prepolymer tubular reactor to be 68 +/-2 ℃, and controlling the retention time of the mixture in the prepolymer tubular reactor to be 20-30 min;
4) then continuously conveying the mixture to a reaction kettle by a high-viscosity pump, controlling the temperature in the reaction kettle to be 84-86 ℃, respectively adding the rest 4,4' -diphenylmethane diisocyanate, the rest xylylene diisocyanate and an organic bismuth catalyst, and reacting until the measured value of the NCO value is 0.35-0.40 percent after the addition is finished;
5) respectively adding isophorone diamine and KH-560 into the reaction kettle, controlling the temperature in the reaction kettle to be 76-78 ℃ after the addition is finished, and carrying out heat preservation reaction for 3-4 hours;
6) stopping heating, adding the organic silicon anti-sticking agent, continuously stirring for 20-40 min, and discharging to obtain the high-stripping hydrolysis-resistant polyurethane resin;
the whole reaction process in the reaction kettle is nitrogen atmosphere, and a nitrogen charging device is adopted to charge nitrogen into the reaction kettle.
The polyurethane production equipment comprises a mixing and stirring kettle, a feeding device, a prepolymer tubular reactor, a heating reaction kettle, a nitrogen filling device, a high viscosity pump and a finished product tank;
the mixing and stirring kettle, the feeding device, the prepolymer tubular reactor, the heating reaction kettle and the finished product tank are sequentially communicated through pipelines;
high-viscosity pumps are arranged on pipelines between the prepolymer tubular reactor and the heating reaction kettle and between the heating reaction kettle and the finished product tank; the heating reaction kettle is communicated with a nitrogen charging device.
In practical application, the high-peel hydrolysis-resistant polyurethane resin can be obtained by selectively adding a solvent or other diluents, diluting the high-peel hydrolysis-resistant polyurethane resin, and then discharging the diluted high-peel hydrolysis-resistant polyurethane resin to a finished product tank through a high-viscosity pump; if the viscosity of the high-peel hydrolysis-resistant polyurethane resin is too high and dilution is not needed, the high-viscosity polyurethane resin is difficult to discharge to a finished product tank through a high-viscosity pump, the high-peel hydrolysis-resistant polyurethane resin can be discharged through a turnover heating reaction kettle, and specific technicians in the field can select and operate the high-peel hydrolysis-resistant polyurethane resin according to actual needs.
The polyurethane production equipment disclosed by the invention is relatively simple in integral structure and convenient to use, realizes continuous production of polyurethane, is small and medium-sized equipment capable of realizing continuous production, and can well combine mixing, feeding, pre-polymerization, discharging and storage to form complete continuous polyurethane production equipment; the devices/equipment of the polyurethane production equipment in the links of mixing, feeding, prepolymerization, polymerization, discharging, storage and the like are well designed and adjusted, so that the requirements of polyurethane production can be well met, and the quality of the produced polyurethane is effectively ensured.
Preferably, the mixing and stirring kettle comprises a kettle body, wherein the inner wall of the kettle body is fixedly connected with two fixing frames which are parallel to each other, one opposite sides of the two fixing frames are fixedly connected with a fixing pipe together, the inner center position of the kettle body is fixedly connected with a triangular support, the top of the triangular support is rotatably connected with a main shaft, the fixing pipe and the kettle body are rotatably connected with stirring rods together, the number of the stirring rods is four, the number of the stirring rods is symmetrical to each other, the outer surfaces of the four stirring rods are fixedly connected with stirring blades, one end of each stirring rod is fixedly connected with a second helical gear, the second helical gear is positioned in the fixing pipe, the outer surface of the main shaft is fixedly connected with a first helical gear corresponding to the position of the second helical gear, the first helical gear is meshed with the second helical gear, one end of the main shaft, which is far away, a kettle cover is arranged at the top of the kettle body, a servo motor is fixedly connected to the center of the top of the kettle cover, an output shaft of the servo motor is fixedly connected with a rotary rod, and the rotary rod is in through connection with the kettle cover;
preferably, the feeding device comprises a base, a first groove is formed in the upper surface of the base, a bidirectional threaded rod is rotatably connected inside the first groove, two threaded blocks are sleeved on the outer surface of the bidirectional threaded rod, two rotating rods are rotatably connected to the top ends of the two threaded blocks, the middle positions of the two rotating rods are in cross rotating connection, a lifting plate is arranged above the two rotating rods, a second groove is formed in the lower surface of the lifting plate, a fixing rod is fixedly connected inside the second groove, two sliding sleeves are sleeved on the outer surface of the fixing rod, one ends of the two rotating rods, which are far away from the two threaded blocks, are respectively rotatably connected with the bottom ends of the two sliding sleeves, a feeding pump, a fixing box and a liquid storage box are respectively and fixedly connected to the upper surface of the lifting plate, and a feeding pipe is connected to the material suction end of the feeding pump, the discharging pipe is connected with a discharging pipe through a pipe at the discharging end of the feeding pump, one end, away from the feeding pump, of the discharging pipe extends into the fixed box and extends out of the top wall of the fixed box, a semiconductor refrigerating sheet is fixedly embedded at the top of the liquid storage box, a radiating sheet is fixedly connected at the hot end of the semiconductor refrigerating sheet, a cold guide sheet is fixedly connected at the cold end of the semiconductor refrigerating sheet, a water pump is fixedly connected with the inner wall of the liquid storage box, a water outlet end pipe of the water pump is connected with a cold water pipe, one end, away from the water pump, of the cold water pipe extends to the inside of the fixed box and is spirally wound on the outer surface of the discharging pipe, and one;
preferably, the prepolymer tubular reactor comprises a tube body, a first material receiving tube and a second material receiving tube are respectively arranged on two sides of the top end of the tube body, a material pump is fixedly connected to the outer side wall of the tube body, a return pipe is fixedly connected at the bottom end of the pipe body, a first electromagnetic valve is arranged on one side of the return pipe close to the pipe body, one side of the bottom end of the return pipe is fixedly connected with a driving motor, an output shaft of the driving motor penetrates through the outer side wall of the return pipe to extend to the inner side and is fixedly connected with a stirring impeller, the top end of the return pipe is fixedly connected with the top of the pipe body, a second electromagnetic valve is arranged at the position of the return pipe close to the top of the pipe body, the heating pads are nested on the outer side walls of the return pipe and the pipe body, a material storage tank is fixedly connected to one side, close to the return pipe, of the bottom end of the pipe body, and a third electromagnetic valve is arranged on one side, close to the material storage tank, of the bottom end of the pipe body;
preferably, the heating reaction kettle comprises a bottom plate and a reaction container; the middle part of the top surface of the bottom plate is fixedly provided with an electric heating plate, the top end of the electric heating plate is fixedly connected with a heat exchange barrel, a heating part of the electric heating plate penetrates through the bottom surface of the heat exchange barrel to the bottom end of the inner cavity of the heat exchange barrel, an inner cavity of the heat exchange barrel is filled with a heat exchange medium, the top surface of the heat exchange barrel is fixedly connected with an annular cover, four corners of the top surface of the bottom plate are fixedly connected with electric support rods, the top ends of the electric support rods on the same side are fixedly connected with support cross rods, the middle parts of the support cross rods are rotatably connected with annular cross arms, the middle parts of the annular cross arms are embedded and fixed with the outer wall of the reaction container, the bottom end of the reaction container penetrates through a center hole of the annular cover to the inner cavity of the heat exchange barrel, an output shaft of the motor is fixedly connected with a driving pinion, and the driving pinion is meshed with a turnover gear;
preferably, the nitrogen charging device comprises a device body; the inner side wall of the device main body is fixedly connected with a partition plate, the inner bottom wall of the device main body is provided with a nitrogen storage bottle, the bottom of the partition plate is fixedly connected with a first connecting pipe, the end part of the nitrogen storage bottle is fixedly connected with a second connecting pipe, the surfaces of the first connecting pipe and the second connecting pipe are both fixedly connected with a connecting ring, the surface of the second connecting pipe is fixedly connected with a supporting plate, the top of the supporting plate is fixedly connected with a supporting spring, the top of the supporting spring is fixedly connected with a connecting rod, the bottom of the connecting rod is fixedly connected with an inserting rod, the inserting rod is in penetrating connection with the connecting ring, the bottom of the device main body is fixedly connected with a base, the top of the base is provided with a special-shaped groove, the bottom of the device main body;
preferably, the high viscosity pump includes a motor, a pump body housing, and a mounting plate; the outer fixed surface of motor is connected with the connecting plate, spacing jack has all been seted up on the both sides surface of connecting plate, the bar groove has been seted up to the upper end surface of motor, the inside fixedly connected with dead lever in bar groove, the surface cover of dead lever is equipped with the spring, the surface sliding connection of dead lever has the movable block, the spacing inserted bar of one side fixedly connected with of movable block, the upper end surface of movable block has seted up the knot and has moved the hole, the upper end fixedly connected with protecting crust of mounting panel, the output fixed mounting of motor has the shaft coupling.
Preferably, the center positions of the outer surfaces of the two fixing frames are provided with openings, the two fixing frames are communicated with the fixing pipe through the openings, and the spindle is in penetrating connection with the fixing frames and the fixing pipe.
Preferably, a hexagonal nut is arranged between the kettle body and the kettle cover, and the kettle body is fixedly connected with the kettle cover through the hexagonal nut.
Preferably, the outer surfaces of the two fixing frames are provided with openings.
Preferably, the surface of one end of rotary rod is provided with square constant head tank, and square locating piece and square constant head tank embedding are connected.
Preferably, the bottom of the kettle body is provided with a discharge hole, and the top of the kettle cover is provided with a feed hole.
Preferably, one end of the bidirectional threaded rod penetrates through the side wall of the first groove and extends to the outside of the base, and a crank is fixedly connected with the outside of the base.
Preferably, the upper surface of the base is fixedly connected with four guide rods, and the top ends of the four guide rods penetrate through the side wall of the lifting plate and extend to the outside.
Preferably, the inside of the liquid storage tank is provided with circulating cold water.
Preferably, the upper surface of the heat sink is fixedly connected with a heat dissipation fan.
Preferably, the cold guide plate extends to the inside of the liquid storage tank.
Preferably, a feeding port is arranged at the position, close to the first electromagnetic valve, of the bottom end of the return pipe.
Preferably, the bottom end of the storage tank is provided with a discharge hole.
Preferably, the inner sides of the feeding port and the discharging port are provided with fourth electromagnetic valves.
Preferably, one side of the inner side wall of the pipe body, which is close to the first material receiving pipe and the second material receiving pipe, is provided with a coarse dredging net, one side of the inner side wall of the pipe body, which is far away from the first material receiving pipe and the second material receiving pipe, is provided with a fine dredging net, and the top end of the return pipe is located on the top side of the coarse dredging net.
Preferably, the material pump is positioned at the middle side between the coarse dredging net and the fine dredging net.
Preferably, one side fixed mounting of bottom plate has an electric cabinet, fixed mounting has automatic temperature controller, motor drive and power controller in the electric cabinet, automatic temperature controller electric connection motor drive and power controller's control end, motor drive electric connection motor and four electric support poles, power controller electric connection electric heating plate.
Preferably, the inner bottom wall of the reaction vessel is fixedly connected with a heat conduction column, and the heat conduction column extends to the middle part of the inner cavity of the reaction vessel.
Preferably, the inner cavity of the heat exchange barrel is fixedly connected with a first thermal sensor, the inner cavity of the reaction container is fixedly connected with a second thermal sensor, and the first thermal sensor and the second thermal sensor are both electrically connected with a signal end of the automatic temperature controller.
Preferably, the electric heating plate is a resistor type or a capacitor type, and the reaction vessel is made of stainless steel material.
Preferably, the inner bottom wall of the device main body is fixedly connected with a fixing plate, the side edge of the fixing plate is fixedly connected with a clamping spring, the end part of the clamping spring is fixedly connected with a clamping plate, and the clamping plate is in contact with the nitrogen storage bottle.
Preferably, the top of base is provided with the bolt, the screw hole has been seted up to the bottom in dysmorphism groove, the bolt runs through dysmorphism board and screw hole threaded connection.
Preferably, the surface of the device main body is rotatably connected with a device door through a hinge, and the side edge of the device main body is fixedly connected with an air outlet pipe.
Preferably, the top of the supporting plate is fixedly connected with a guide rod, and the guide rod is in through connection with the connecting rod.
Preferably, the top of the connecting rod is fixedly connected with a handle, and the surface of the first connecting pipe is provided with an electromagnetic valve.
Preferably, the upper end of the protective shell is provided with a top cover, the upper end of the top cover is in threaded connection with a fastening screw, the upper end of the protective shell is provided with a threaded hole, and the lower end of the mounting plate is fixedly connected with an elastic rubber block.
Preferably, the pump body shell comprises a wear-resistant layer, a corrosion-resistant layer is fixedly bonded on the outer surface of the wear-resistant layer, and a high-temperature-resistant layer is fixedly bonded on the outer surface of the corrosion-resistant layer.
Preferably, the wear-resistant layer is made of an ultra-high molecular weight polyethylene material, the corrosion-resistant layer is made of a polytetrafluoroethylene material, and the high-temperature-resistant layer is made of a polyurethane material.
Preferably, one end of the spring is fixedly connected with the inner side wall of the strip-shaped groove, and the other end of the spring is fixedly connected with the surface of one side of the moving block.
Preferably, one end of the limiting insertion rod is inserted into the inner wall of the limiting insertion hole, and the opening diameter of the limiting insertion hole is matched with the design diameter of one end of the limiting insertion rod.
Compared with the prior art, the invention has the following advantages and beneficial effects:
the high-stripping hydrolysis-resistant polyurethane resin is prepared by selecting raw materials, optimizing the content of each raw material, selecting 1, 6-hexanediol adipate, polytetrahydrofuran diol PTMEG-3000, polyethylene glycol, trimethylolpropane, 4' -diphenylmethane diisocyanate, xylylene diisocyanate, an organic bismuth catalyst, isophorone diamine, KH-560 and an organic silicon anti-sticking agent in a proper proportion, and distributing the advantages of each raw material, wherein the raw materials are matched with each other and are mutually promoted, and the high-stripping hydrolysis-resistant polyurethane resin obtained by polymerization has high stripping strength, good hydrolysis resistance and high stripping and hydrolysis resistance; the high-peel hydrolysis-resistant polyurethane resin can be directly coated on a textile fabric or a non-woven fabric, so that the high-peel hydrolysis-resistant polyurethane resin has high peel and good hydrolysis resistance after film formation, and a coated textile fabric or non-woven fabric finished product also has high peel and good hydrolysis resistance.
The synthetic leather prepared by the conventional polyester resin has the advantages that after being soaked in a 10% sodium hydroxide solution for 12 hours, the surface of the leather is pulverized, and the peel strength is not high; after the synthetic leather prepared from the high-peel hydrolysis-resistant polyurethane resin is soaked in a 10% sodium hydroxide solution for 12 hours, the peel strength can reach 81.6% relative to the original peel retention rate.
The high-stripping hydrolysis-resistant polyurethane resin is produced by adopting special polyurethane production equipment, the polyurethane production equipment is relatively simple in integral structure and convenient to use, the continuous production of polyurethane is realized, and the high-stripping hydrolysis-resistant polyurethane resin is small and medium-sized equipment capable of continuously producing, can well combine material mixing, feeding, pre-polymerization, discharging and storage to form complete continuous polyurethane production equipment; the devices/equipment of the polyurethane production equipment in the links of mixing, feeding, prepolymerization, polymerization, discharging, storage and the like are well designed and adjusted, so that the requirements of polyurethane production can be well met, and the quality of the produced polyurethane is effectively ensured. Greatly improves the production efficiency of polyurethane, reduces the labor intensity of workers, and can effectively ensure the quality of the produced polyurethane.
In addition, the polyurethane production equipment disclosed by the invention is convenient for realizing automatic control and is beneficial to realizing continuous automatic production.
1. When the mixing and stirring kettle is used, the servo motor is firstly turned on, the servo motor can drive the rotary rod to rotate, the rotary rod can drive the main shaft to rotate through the square positioning block and the square positioning groove, the main shaft can drive the first bevel gears to rotate, the first bevel gears can simultaneously drive the second bevel gears to rotate, the second bevel gears can drive the stirring rod to rotate at a fixed position, and the stirring rod can drive the stirring blades to rotate, so that the stirring blades can stir liquid in the kettle body.
2. According to the feeding device, the lifting plate can be lifted only by rotating the crank through the arrangement of the bidirectional threaded rod, the rotating rod, the threaded block, the sliding sleeve, the fixed rod, the guide rod, the lifting plate and the crank, so that the height of the device can be adjusted conveniently, and the device can be fed according to the heights of different stirring barrels. Through the setting of liquid reserve tank, semiconductor refrigeration piece, water pump, cold water pipe, lead cold piece, fin, be convenient for cool down the raw materials through hydrologic cycle at the in-process of material loading to further reduce the inside temperature of liquid reserve tank through the semiconductor refrigeration piece, make the cooling effect better, in order to avoid material temperature high temperature, influence the raw materials chemical property and taken place. The device is convenient for adjusting the height of the device to meet the requirements of mixing tanks with different heights, and can cool the raw materials in the feeding process, thereby avoiding influencing the chemical properties of the raw materials.
3. According to the prepolymer tubular reactor, materials entering a tube body sequentially pass through a coarse dredging net and a fine dredging net under the driving of a material pump, so that the materials are sequentially filtered to avoid the situation that the materials are blocked in the tube body, then, a first electromagnetic valve is opened to enable the materials in the tube body to flow into a return pipe, a fourth electromagnetic valve on a feeding port is opened to enable the mixed materials to be conveyed into the return pipe, meanwhile, a driving motor drives a stirring impeller to rotate to mix the mixed materials with the materials, then, a second electromagnetic valve is opened to enable the mixed materials to flow back into the tube body, so that the mixed materials are fully mixed through circular flow, in the process, a heating pad supplies heat to the whole mixing and reaction process, the mixing and reaction speed is improved, and meanwhile, the occupied space of the whole device can be saved.
4. According to the heating reaction kettle, the electric support rods are arranged to alternately stretch and retract to drive the reaction container to intermittently contact with the electric heating plate, so that the electric heating plate directly heats the reaction container, the temperature is rapidly increased, when the direct heating reaches the set temperature, the electric support rods push the reaction container to rise to indirectly heat, the continuous temperature and the temperature are obtained, and the reaction stability is enhanced. This heating reation kettle, inner diapire fixedly connected with heat conduction post of reaction vessel, heat conduction post extend to the middle part of reaction vessel inner chamber, can conduct the heat of reaction vessel bottom to reaction vessel's middle part and top rapidly, have avoided by the slow problem of colloidal polyurethane raw materials heat conduction for reaction vessel's inner chamber is in the balanced state of temperature rapidly, thereby promotes polyurethane's preparation quality.
5. According to the nitrogen charging device, the first connecting pipe, the second connecting pipe and the plurality of nitrogen storage bottles are arranged, so that nitrogen can be continuously supplied when the nitrogen charging device is used, the working efficiency is better when the nitrogen charging device is used, and the problem that the nitrogen charging device cannot continuously work when a single nitrogen bottle is replaced when the nitrogen amount is insufficient is solved. This fill nitrogen device makes can be better to the device install fixedly when using and making through the cooperation between dysmorphism groove and the dysmorphism board to it can be more stable firm to make when using.
6. According to the high-viscosity pump, the whole body can be rapidly disassembled when transportation or maintenance is needed through the connecting plate, the limiting insertion holes and the limiting insertion rods, so that the single body can be detached, targeted maintenance is facilitated, rapid assembly can be performed after transportation, and equipment can be put into use at the first time. This high viscosity pump passes through wearing layer, corrosion-resistant layer and high temperature resistant layer to let the pump body shell possess better wear-resisting, corrosion-resistant and high temperature resistant performance, increased holistic life.
Drawings
FIG. 1 is a schematic structural view of the present invention;
FIG. 2 is a schematic diagram of the overall structure of the mixing and stirring tank of the present invention;
FIG. 3 is an enlarged view of B of FIG. 2 in accordance with the present invention;
FIG. 4 is a schematic structural view of the fixing frame according to the present invention;
FIG. 5 is a schematic view of the connection between the rotating rod and the spindle according to the present invention;
FIG. 6 is a main sectional view of the loading device of the present invention;
FIG. 7 is a partial side view of the loading device of the present invention;
FIG. 8 is a cross-sectional view of a reservoir of the loading device of the present invention;
FIG. 9 is a schematic view of the overall structure of a tubular prepolymer reactor according to the present invention;
FIG. 10 is a schematic view of the internal structure of a tubular body of a tubular reactor for a prepolymer according to the present invention;
FIG. 11 is a schematic view of the internal structure of a reflux pipe of the prepolymer tubular reactor of the present invention;
FIG. 12 is a schematic view of a side structure of a heating reactor according to the present invention;
FIG. 13 is a schematic view of another side of the heating reactor according to the present invention;
FIG. 14 is a schematic side sectional view of a heated reactor according to the present invention;
FIG. 15 is a schematic structural view of a nitrogen charging apparatus according to the present invention;
FIG. 16 is a schematic structural diagram of the main body of the nitrogen charging device according to the present invention;
FIG. 17 is a schematic view of the connection of a first connection pipe and a second connection pipe of the nitrogen charging device according to the present invention;
FIG. 18 is a schematic view of the construction of a high viscosity pump according to the present invention;
FIG. 19 is an enlarged view of the structure of FIG. 18 at A in accordance with the present invention;
fig. 20 is a schematic structural layer of a pump body casing of the high viscosity pump of the present invention.
In the figure: 1. mixing and stirring the mixture in a kettle; 2. a feeding device; 3. a prepolymer tubular reactor; 4. heating the reaction kettle; 5. a nitrogen charging device; 6. a high viscosity pump; 7. A finished product tank;
101. a kettle body; 102. a kettle cover; 103. a hexagonal nut; 104. a servo motor; 105. rotating the rod; 106. a fixed tube; 107. a fixed mount; 108. a main shaft; 109. a stirring rod; 1010. stirring blades; 1011. a first helical gear; 1012. a second helical gear; 1013. an opening; 1014. opening a hole; 1015. a square positioning block; 1016. a square positioning groove; 1017. a triangular bracket;
201. a base; 202. a first groove; 203. a bidirectional threaded rod; 204. a thread block; 205. rotating the rod; 206. a lifting plate; 207. a guide bar; 208. A crank; 209. a second groove; 2010. fixing the rod; 2011. a sliding sleeve; 2012. a feeding pump; 2013. a feed pipe; 2014. a discharge pipe; 2015. a fixed box; 2016. a cold water pipe; 2017. a liquid storage tank; 2018. a water pump; 2019. a semiconductor refrigeration sheet; 2020. a heat sink; 2021. a heat radiation fan; 2022. A cold conducting sheet;
301. a pipe body; 302. a first material receiving pipe; 303. a second material receiving pipe; 304. a heating pad; 305. a material pump; 306. a return pipe; 307. a first solenoid valve; 308. coarse mesh thinning; 309. finely thinning the net; 3010. a second solenoid valve; 3011. a drive motor; 3012. a stirring impeller; 3013. a feeding port; 3014. a third electromagnetic valve; 3015. a material storage tank; 3016. a discharge port; 3017. a fourth solenoid valve;
401. a base plate; 402. an electric heating plate; 403. a heat exchange tub; 404. an annular cover; 405. an electric support bar; 406. a support rail; 407. an annular cross arm; 408. a reaction vessel; 409. turning over the gear; 4010. an electric motor; 4011. a drive pinion; 4012. an electric cabinet; 4013. an automatic temperature controller; 4014. A motor driver; 4015. a power controller; 4016. a heat-conducting column; 4017. a first thermal sensor; 4018. a second thermal sensor;
501. a device main body; 502. a partition plate; 503. storing a nitrogen bottle; 504. a first connecting pipe; 505. a second connecting pipe; 506. a connecting ring; 507. a support plate; 508. a support spring; 509. a connecting rod; 5010. inserting a rod; 5011. a base; 5012. a special-shaped groove; 5013. a shaped plate; 5014. a fixing plate; 5015. A clamping spring; 5016. a clamping plate; 5017. a bolt; 5018. a threaded hole; 5019. a device door; 5020. an air outlet pipe; 5021. a guide bar; 5022. a handle;
601. an electric motor; 602. a pump body housing; 6021. a wear layer; 6022. a corrosion-resistant layer; 6023. a high temperature resistant layer; 603. mounting a plate; 604. a connecting plate; 605. limiting the jacks; 606. a strip-shaped groove; 607. fixing the rod; 608. a spring; 609. a moving block; 6010. a limiting inserted rod; 6011. buckling holes; 6012. A protective shell; 6013. a coupling; 6014. a top cover; 6015. fastening screws; 6016. a threaded hole; 6017. an elastic rubber block.
Detailed Description
In order that those skilled in the art will better understand the technical solutions of the present invention, the following description of the preferred embodiments of the present invention is provided in conjunction with specific examples, but it should be understood that the drawings are for illustrative purposes only and should not be construed as limiting the patent; for the purpose of better illustrating the embodiments, certain features of the drawings may be omitted, enlarged or reduced, and do not represent the size of an actual product; it will be understood by those skilled in the art that certain well-known structures in the drawings and descriptions thereof may be omitted. The positional relationships depicted in the drawings are for illustrative purposes only and are not to be construed as limiting the present patent.
Example 1:
the high-peel hydrolysis-resistant polyurethane resin is prepared from the following raw materials in parts by weight: poly (1, 6-hexanediol adipate) glycol: 15-25 parts of polytetrahydrofuran diol PTMEG-3000: 20-27 parts of polyethylene glycol: 50-70 parts of trimethylolpropane: 5.5-8.5 parts of 4,4' -diphenylmethane diisocyanate: 10-12 parts of xylylene diisocyanate: 5-6.5 parts of organic bismuth catalyst: 0.2-0.35 parts of isophorone diamine: 3.5-4.5 parts of KH-560: 2.5-3.5 parts of an organic silicon anti-sticking agent: 0.5-0.8 part; the molecular weight of the poly adipic acid 1, 6-hexanediol glycol ester is 1500-2000; the molecular weight of the polyethylene glycol is 2000-2500; the mixture of the organosilicon antisticking agent AC-1800K and the antisticking agent FY-5080K is prepared from the following components in a mass ratio of 1: 0.75 to 0.88.
The invention also provides a preparation method of the high-peel hydrolysis-resistant polyurethane resin, which adopts polyurethane production equipment to carry out continuous production preparation and comprises the following steps:
1) weighing the raw materials of the aliphatic non-yellowing polyurethane resin according to the parts by weight;
2) putting poly adipic acid 1, 6-hexanediol glycol, polytetrahydrofuran diol PTMEG-3000, polyethylene glycol, trimethylolpropane, 1/2 4,4' -diphenylmethane diisocyanate and 1/2 xylylene diisocyanate into a mixing and stirring kettle (1), and uniformly mixing to obtain a mixture;
3) conveying the mixture into a prepolymer tubular reactor (3) by using a feeding device (2), and carrying out prepolymerization, wherein the temperature in the prepolymer tubular reactor (3) is controlled to be 68 +/-2 ℃, and the retention time of the mixture in the prepolymer tubular reactor (3) is controlled to be 20-30 min;
4) then continuously conveying the mixture into a reaction kettle (4) through a high-viscosity pump (6), controlling the temperature in the reaction kettle (4) to be 84-86 ℃, respectively adding the rest 4,4' -diphenylmethane diisocyanate, the rest xylylene diisocyanate and an organic bismuth catalyst, and reacting until the measured value of NCO value is 0.35-0.40% after the addition is finished;
5) respectively adding isophorone diamine and KH-560 into the reaction kettle (4), controlling the temperature in the reaction kettle (4) to be 76-78 ℃ after the addition is finished, and carrying out heat preservation reaction for 3-4 h;
6) stopping heating, adding the organic silicon anti-sticking agent, continuously stirring for 20-40 min, and discharging to obtain the high-stripping hydrolysis-resistant polyurethane resin;
the whole reaction process in the reaction kettle (4) is in a nitrogen atmosphere, and a nitrogen charging device (5) is adopted to charge nitrogen into the reaction kettle (4).
Example 2:
the high-peel hydrolysis-resistant polyurethane resin is prepared from the following raw materials in parts by weight: poly (1, 6-hexanediol adipate) glycol: 15 parts of polytetrahydrofuran diol PTMEG-3000: 20 parts of polyethylene glycol: 50 parts of trimethylolpropane: 5.5 parts of 4,4' -diphenylmethane diisocyanate: 10 parts of xylylene diisocyanate: 5 parts of organic bismuth catalyst: 0.2 part of isophorone diamine: 3.5 parts, KH-560: 2.5 parts of organosilicon antisticking agent: 0.5 part; the molecular weight of the poly adipic acid 1, 6-hexanediol glycol ester diol is 1500-2000; the molecular weight of the polyethylene glycol is 2000-2500; the mixture of the organosilicon antisticking agent AC-1800K and the antisticking agent FY-5080K is prepared from the following components in a mass ratio of 1: 0.75.
in this embodiment, the preparation method of the high-peel hydrolysis-resistant polyurethane resin adopts polyurethane production equipment to perform continuous production and preparation, and includes the following steps:
1) weighing the raw materials of the aliphatic non-yellowing polyurethane resin according to the parts by weight;
2) putting poly adipic acid 1, 6-hexanediol glycol, polytetrahydrofuran diol PTMEG-3000, polyethylene glycol, trimethylolpropane, 1/2 4,4' -diphenylmethane diisocyanate and 1/2 xylylene diisocyanate into a mixing and stirring kettle (1), and uniformly mixing to obtain a mixture;
3) conveying the mixture into a prepolymer tubular reactor (3) by using a feeding device (2), carrying out prepolymerization, controlling the temperature in the prepolymer tubular reactor (3) to be 66 ℃, and controlling the retention time of the mixture in the prepolymer tubular reactor (3) to be 30 min;
4) then continuously conveying the mixture into a reaction kettle (4) through a high-viscosity pump (6), controlling the temperature in the reaction kettle (4) to be 84 ℃, respectively adding the rest 4,4' -diphenylmethane diisocyanate, the rest xylylene diisocyanate and an organic bismuth catalyst, and reacting until the measured value of the NCO value is 0.40 percent after the addition is finished;
5) respectively adding isophorone diamine and KH-560 into the reaction kettle (4), controlling the temperature in the reaction kettle (4) to be 76 ℃ after the addition is finished, and carrying out heat preservation reaction for 4 hours;
6) stopping heating, adding the organic silicon anti-sticking agent, continuously stirring for 40min, and discharging to obtain the high-stripping hydrolysis-resistant polyurethane resin;
the whole reaction process in the reaction kettle (4) is in a nitrogen atmosphere, and a nitrogen charging device (5) is adopted to charge nitrogen into the reaction kettle (4).
In this embodiment, as shown in fig. 1 to 20, the adopted polyurethane production equipment includes a mixing and stirring tank 1 for mixing (part/all) raw materials for polyurethane production, and a feeding device 2 for feeding (part/all) raw materials for polyurethane production, or feeding; in the actual use process, a plurality of feeding devices 2 can be arranged as necessary, and different raw materials can be added according to the needs, which can be understood by those skilled in the art. The prepolymer tubular reactor 3 is used for pre-polymerizing (partial/total) raw materials for producing polyurethane, the heating reaction kettle 4 is used for main reactions such as polymerization reaction, broad chain and the like of polyurethane, a polyurethane product is obtained by discharging, the nitrogen filling device 5, the high viscosity pump 6 is used for circulating and pressurizing high-viscosity liquid or solid-liquid mixture, and the finished product tank 7 is used for storing the polyurethane product discharged from the heating reaction kettle 4;
the mixing and stirring kettle 1, the feeding device 2, the prepolymer tubular reactor 3, the heating reaction kettle 4 and the finished product tank 7 are communicated in sequence through pipelines;
a high-viscosity pump 6 is arranged on a pipeline between the prepolymer tubular reactor 3 and the heating reaction kettle 4 and a pipeline between the heating reaction kettle 4 and the finished product tank 7;
the heating reaction kettle 4 is communicated with a nitrogen charging device 5; the nitrogen charging device 5 charges nitrogen into the heating reaction kettle 4 to ensure that the heating reaction kettle 4 is in nitrogen atmosphere when needed (in the projection process).
The mixing and stirring kettle 1 comprises a kettle body 101, wherein the inner wall of the kettle body 101 is fixedly connected with two fixing frames 107, the fixing frames 107 are parallel to each other, one opposite sides of the two fixing frames 107 are fixedly connected with a fixing pipe 106 together, the inner center position of the kettle body 101 is fixedly connected with a triangular bracket 1017, the top of the triangular bracket 1017 is rotatably connected with a main shaft 108, the fixing pipe 106 and the kettle body 101 are rotatably connected with stirring rods 109 together, the stirring rods 109 are four symmetrical to each other, the outer surfaces of the four stirring rods 109 are fixedly connected with stirring blades 1010, one end of each stirring rod 109 is fixedly connected with a second bevel gear 1012, the second bevel gear 1012 is positioned inside the fixing pipe 106, the outer surface of the main shaft 108 is fixedly connected with a first bevel gear 1011 corresponding to the position of the second bevel gear 1012, the first bevel gear 1011 is meshed with the second bevel gear 1012, one end of the main shaft 108 far away from the triangular bracket 101, the top of the kettle body 101 is provided with a kettle cover 102, the top center position of the kettle cover 102 is fixedly connected with a servo motor 104, the output shaft of the servo motor 104 is fixedly connected with a rotary rod 105, and the rotary rod 105 is in through connection with the kettle cover 102.
The center positions of the outer surfaces of the two fixing frames 107 are respectively provided with an opening 1014, the two fixing frames 107 are communicated with the fixing pipe 106 through the openings 1014, and the main shaft 108 is in through connection with the fixing frames 107 and the fixing pipe 106, so that the main shaft 108 can drive the stirring blades 1010 to perform rotary stirring; the hexagonal nuts 103 are commonly arranged between the kettle body 101 and the kettle cover 102, and the kettle body 101 is fixedly connected with the kettle cover 102 through the hexagonal nuts 103, so that the kettle cover 102 can be conveniently opened from the upper surface of the kettle body 101, and the interior of the kettle body 101 can be conveniently cleaned; the outer surfaces of the two fixing frames 107 are provided with openings 1013 which can facilitate the flow of the liquid in the kettle body 101; the outer surface of one end of the rotating rod 105 is provided with a square positioning groove 1016, and the square positioning block 1015 is connected with the square positioning groove 1016 in an embedded manner, so that the rotating rod 105 can drive the spindle 108 to rotate, and meanwhile, the installation and butt joint are facilitated; the bottom of the kettle body 101 is provided with a discharge hole, and the top of the kettle cover 102 is provided with a feed hole, so that feeding and discharging can be facilitated.
The feeding device 2 comprises a base 201, a first groove 202 is formed in the upper surface of the base 201, a bidirectional threaded rod 203 is rotatably connected inside the first groove 202, two threaded blocks 204 are sleeved on the outer surface threads of the bidirectional threaded rod 203, two rotating rods 205 are rotatably connected to the top ends of the two threaded blocks 204, the middle positions of the two rotating rods 205 are in cross rotating connection, a lifting plate 206 is arranged above the two rotating rods 205, a second groove 209 is formed in the lower surface of the lifting plate 206, a fixing rod 2010 is fixedly connected inside the second groove 209, two sliding sleeves 2011 are sleeved on the outer surface of the fixing rod 2010, one ends of the two rotating rods 205, which are far away from the two threaded blocks 204, are respectively rotatably connected with the bottom ends of the two sliding sleeves 2011, a feeding pump 2012, a fixing box 2015 and a liquid storage box 2017 are respectively fixedly connected to the upper surface of the lifting plate 206, a feeding end pipe 201, the discharging end of the feeding pump 2012 is connected with a discharging pipe 2014, one end of the discharging pipe 2014, which is far away from the feeding pump 2012, extends to the inside of the fixed box 2015 and extends out of the top wall of the fixed box 2015, the top of the liquid storage box 2017 is fixedly connected with a semiconductor refrigeration sheet 2019 in an embedded mode, the hot end of the semiconductor refrigeration sheet 2019 is fixedly connected with a radiating fin 2020, the cold end of the semiconductor refrigeration sheet 2019 is fixedly connected with a cold guide sheet 2022, the inner wall of the liquid storage box 2017 is fixedly connected with a water pump 2018, the water outlet end of the water pump 2018 is connected with a cold water pipe 2016, one end of the cold water pipe 2016, which is far away from the water pump 2018, extends to the outer surface of the discharging pipe 2014 in a spiral winding mode inside the.
One end of the bidirectional threaded rod 203 penetrates through the side wall of the first groove 202 and extends to the outside of the base 201 to be fixedly connected with a crank 208, so that the bidirectional threaded rod 203 can be conveniently rotated; the upper surface of the base 201 is fixedly connected with four guide rods 207, and the top ends of the four guide rods 207 penetrate through the side wall of the lifting plate 206 and extend to the outside, so that the lifting stability of the lifting plate 206 is improved; circulating cold water is arranged in the liquid storage tank 2017 so as to cool the raw materials; the upper surface of the radiating fin 2020 is fixedly connected with a radiating fan 2021, so that the refrigerating effect of the semiconductor refrigerating fin 2019 is improved; cold guide 2022 extends to the interior of reservoir 2017 to cool the water in reservoir 2017.
Prepolymer tubular reactor 3 includes body 301, the top both sides of body 301 are provided with first material receiving pipe 302 and second material receiving pipe 303 respectively and are connected with material pump 305 to the lateral wall fixedly connected with of body 301, the bottom fixedly connected with back flow pipe 306 of body 301, one side that back flow pipe 306 is close to body 301 is provided with first solenoid valve 307, one side fixedly connected with driving motor 3011 of the bottom of back flow pipe 306, driving motor 3011's output shaft runs through the lateral wall that back flow pipe 306 and extends to inboard and fixedly connected with stirring impeller 3012, the top of back flow pipe 306 and the top fixed connection of body 301, the position that back flow pipe 306 is close to body 301 top is provided with second solenoid valve 3010, back flow pipe 306 and the equal nested heating pad 304 that is provided with of body 301's lateral wall, one side fixedly connected with storage tank 3015 that the bottom of body 301 is close to back flow pipe 306, one side that the bottom of body.
A feeding port 3013 is arranged at the bottom end of the return pipe 306 near the first electromagnetic valve 307, so that the mixture can be added conveniently; a discharge port 3016 is arranged at the bottom end of the material storage tank 3015, so that the reacted materials can be discharged conveniently; the inner sides of the feeding port 3013 and the discharging port 3016 are respectively provided with a fourth electromagnetic valve 3017, which is convenient for controlling the addition of the mixture and the discharge of the material; a coarse dredging net 308 is arranged on one side, close to the first material receiving pipe 302 and the second material receiving pipe 303, of the inner side wall of the pipe body 301, a fine dredging net 309 is arranged on one side, far away from the first material receiving pipe 302 and the second material receiving pipe 303, of the inner side wall of the pipe body 301, the top end of the return pipe 306 is located on the top side of the coarse dredging net 308, materials entering the pipe body 301 sequentially pass through the coarse dredging net 308 and the fine dredging net 309 under the driving of a material pump 305, and therefore the materials are sequentially filtered to avoid the situation that the materials are blocked in the pipe body 301; the material pump 305 is located at the middle side between the coarse mesh 308 and the fine mesh 309, so as to provide a uniform driving force for the material.
The heating reaction kettle 4 comprises a bottom plate 401 and a reaction vessel 408, an electric heating plate 402 is fixedly installed in the middle of the top surface of the bottom plate 401, a heat exchange barrel 403 is fixedly connected to the top end of the electric heating plate 402, heating elements of the electric heating plate 402 penetrate through the bottom surface of the heat exchange barrel 403 to the bottom end of the inner cavity of the heat exchange barrel, a heat exchange medium is filled in the inner cavity of the heat exchange barrel 403, an annular cover 404 is fixedly connected to the top surface of the heat exchange barrel 403, electric support rods 405 are fixedly connected to four corners of the top surface of the bottom plate 401, support cross rods 406 are fixedly connected to the top ends of the two same-side electric support rods 405, an annular cross arm 407 is rotatably connected to the middle parts of the two support cross arms 406, the outer wall of the reaction vessel 408 is embedded and fixed in the middle part of the annular cross arm 407, the bottom end of the reaction vessel, one side of the support cross bar 406 is fixedly connected with an electric motor 4010, an output shaft of the electric motor 4010 is fixedly connected with a driving pinion 4011, and the driving pinion 4011 is engaged with the overturning gear 409.
In this embodiment, in operation, the electric heating plate 402 is powered on, and after the electric heating plate 402 heats, the heat exchange medium in the inner cavity of the heat exchange barrel 403 is heated, at this time, if the reaction vessel 408 is located at the top end of the inner cavity of the heat exchange barrel 403, the heat exchange medium indirectly heats the reaction vessel 408, and if the electric support rod 405 retracts, the reaction vessel 408 is driven to descend to the top surface of the electric heating plate 402, and at this time, the electric heating plate 402 directly heats the reaction vessel 408; the indirect heating has the advantages of stable temperature, suitability for long-term heating during reaction, rapid direct heating and suitability for the initial stage of reaction, and when the direct heating reaches the set temperature, the electric support rod 405 can push the reaction container 408 to rise for indirect heating; when the polyurethane raw material in the reaction vessel 408 reaches the set temperature, the electric support rod 405 continues to extend forward to push the protruding annular cover 404, at this time, the motor 4010 is started, the motor 4010 is engaged with the overturning gear 409 through the driving pinion 4011, and then the annular cross arm 407 drives the reaction vessel 408 to overturn, so that the polyurethane raw material or the finished product in the reaction vessel 408 is poured out.
Specifically, one side fixed mounting of bottom plate 401 has electric cabinet 4012, fixed mounting has automatic temperature controller 4013, motor driver 4014 and power controller 4015 in electric cabinet 4012, automatic temperature controller 4013 electric connection motor driver 4014 and power controller 4015's control end, motor driver 4014 electric connection motor 4010 and four electric support pole 405, power controller 4015 electric connection electric heating plate 402.
In this embodiment, the automatic temperature controller 4013 adopts a control board containing an MCU chip, and has a program recorded therein, which has signal analysis and operation functions, calculating the input information, comparing the calculation result with the data stored in the calculation result, outputting the transportation result to corresponding instruction and data through the output port of the calculation result, therefore, the output of the motor driver 4014 and the output of the power controller 4015 are controlled according to the heating process, the motor driver 4014 adopts an ASD-B02 type servo driver or a DM860H type stepping driver, the rotating speed and the rotating angle of the motor 4010 can be controlled precisely according to the set pulse current, therefore, the rotation angle of the motor 4010 and the telescopic heights of the four electric support rods 405 are controlled, the power controller 4015 adopts a ZK-3000W type adjustable voltage regulator, and the output power of the electric heating plate 402 can be controlled by adjusting the voltage.
Specifically, the inner bottom wall of the reaction vessel 408 is fixedly connected with a heat conduction column 4016, and the heat conduction column 4016 extends to the middle of the inner cavity of the reaction vessel 408.
In this embodiment, the heat conducting column 4016 is made of a metal tube or a metal rod with good heat conducting property, and can rapidly conduct heat at the bottom end of the reaction container 408 to the middle and the top end of the reaction container 408, thereby avoiding a problem of slow heat conduction by a colloidal polyurethane raw material, so that the inner cavity of the reaction container 408 is rapidly in a state of temperature equilibrium, and improving the preparation quality of polyurethane.
Specifically, a first thermal sensor 4017 is fixedly connected to an inner cavity of the heat exchange barrel 403, a second thermal sensor 4018 is fixedly connected to an inner cavity of the reaction container 408, and the first thermal sensor 4017 and the second thermal sensor 4018 are electrically connected to a signal terminal of the automatic temperature controller 4013.
In this embodiment, the first thermal sensor 4017 and the second thermal sensor 4018 adopt K-type WRNK-191 thermocouples, and the first thermal sensor 4017 and the second thermal sensor 4018 measure the stability of the inner cavity of the heat exchange barrel 403 and the inner cavity of the reaction vessel 408, respectively, so that the power of the electric heating plate 402 is controlled to the optimal reaction temperature of polyurethane by the automatic temperature controller 4013 and the power controller 4015.
Specifically, electric heating plate 402 is resistive or capacitive, and reaction vessel 408 is made of stainless steel.
In this embodiment, the electric heating plate 402 is a resistor or a capacitor, both of which can convert electric energy into heat energy, heat the heat exchange medium contained in the heat exchange barrel 403, or directly heat the bottom end of the reaction vessel 408; the reaction vessel 408 is made of a stainless steel material, has good chemical stability and corrosion resistance, and avoids reacting with raw materials for producing polyurethane.
The automatic temperature controller 4013, the motor driver 4014, the power controller 4015, the first thermal sensor 4017, and the second thermal sensor 4018 in the present embodiment are known technologies that have been disclosed to be widely used in industrial production and daily life.
The nitrogen charging device 5 comprises a device body 501, a partition plate 502 is fixedly connected to the inner side wall of the device body 501, a nitrogen storage bottle 503 is arranged on the inner bottom wall of the device body 501, a first connecting pipe 504 is fixedly connected to the bottom of the partition plate 502, a second connecting pipe 505 is fixedly connected to the end of the nitrogen storage bottle 503, a connecting ring 506 is fixedly connected to the surfaces of the first connecting pipe 504 and the second connecting pipe 505, a supporting plate 507 is fixedly connected to the surface of the second connecting pipe 505, a supporting spring 508 is fixedly connected to the top of the supporting plate 507, a connecting rod 509 is fixedly connected to the top of the supporting spring 508, a plug 5010 is fixedly connected to the bottom of the connecting rod 509, the plug 5010 is in through connection with the connecting ring 506, a base 5011 is fixedly connected to the bottom of the device body 501, a special-shaped groove 5012 is formed in the top of the base 5011, a special-shaped plate 501.
In this embodiment, set up to a plurality ofly through depositing nitrogen bottle 503, and the symmetry sets up for can continuously carry nitrogen gas as required when using, guaranteed the normal use of device, through the setting of baffle 502, carry on spacingly to transport route, make to carry more stable, play the effect of supporting the connection through the setting of backup pad 507, play the fixed effect of connection through connecting rod 509.
Specifically, a fixing plate 5014 is fixedly connected to the inner bottom wall of the apparatus body 501, a clamping spring 5015 is fixedly connected to the side of the fixing plate 5014, a clamping plate 5016 is fixedly connected to the end of the clamping spring 5015, and the clamping plate 5016 is in contact with the nitrogen storage bottle 503.
In this embodiment, the clamping plate 5016 clamps the nitrogen storage bottle 503 by the resilience of the clamping spring 5015, so that the fixing effect is better.
Specifically, a bolt 5017 is arranged at the top of the base 5011, a threaded hole 5018 is formed in the bottom of the special-shaped groove 5012, and the bolt 5017 penetrates through the special-shaped plate 5013 and is in threaded connection with the threaded hole 5018.
In this embodiment, the bolt 5017 is screwed with the threaded hole 5018, so that the special-shaped plate 5013 is limited in the special-shaped slot 5012, thereby achieving the fixing function.
Specifically, the surface of the device body 501 is rotatably connected with a device door 5019 through a hinge, and the side edge of the device body 501 is fixedly connected with an air outlet pipe 5020.
In this embodiment, the nitrogen gas is conveniently conveyed to the external structure when the nitrogen gas is used through the gas outlet pipe 5020.
Specifically, a guide rod 5021 is fixedly connected to the top of the support plate 507, and the guide rod 5021 is connected with the connecting rod 509 in a penetrating manner.
In this embodiment, the guide rod 5021 is convenient to limit the connecting rod 509 when the connecting rod is moved, so that the inserting rod 5010 can better penetrate through the connecting ring 506.
Specifically, a handle 5022 is fixedly connected to the top of the connecting rod 509, and a solenoid valve is mounted on the surface of the first connecting pipe 504.
In this embodiment, the handle 5022 is provided to facilitate pulling the connecting rod 509, and the solenoid valve is provided to facilitate controlling the on/off of the first connecting tube 504.
High viscosity pump 6 includes motor 601, pump body shell 602 and mounting panel 603, motor 601's outer fixed surface is connected with connecting plate 604, spacing jack 605 has all been seted up on the both sides surface of connecting plate 604, bar groove 606 has been seted up to motor 601's upper end surface, the inside fixedly connected with dead lever 607 of bar groove 606, the surface cover of dead lever 607 is equipped with spring 608, the surface sliding connection of dead lever 607 has movable block 609, the spacing inserted bar 6010 of one side fixedly connected with of movable block 609, detain the hole 6011 has been seted up to the upper end surface of movable block 609, the upper end fixedly connected with protecting crust 6012 of mounting panel 603, motor 601's output fixed mounting has shaft coupling 6013.
In this embodiment, when the buckling hole 6011 is loosened, since the moving block 609 presses the spring 608 when moving in the forward stage, after the loosening, the moving block 609 is reset under the rebounding action of the spring 608, so that one end of the limiting insertion rod 6010 is quickly inserted into the inner wall of the limiting insertion hole 605.
Specifically, a top cover 6014 is arranged at the upper end of the protective shell 6012, a fastening screw 6015 is connected to the upper end of the top cover 6014 in a threaded manner, a threaded hole 6016 is formed in the upper end of the protective shell 6012, and an elastic rubber block 6017 is fixedly connected to the lower end of the mounting plate 603.
In this embodiment, the coupler 6013 is placed inside the protective casing 6012 when the motor 601 and the pump casing 602 are connected, and when the protective casing 6012 needs to be repaired or lubricated, the fastening screw 6015 may be loosened by unscrewing, and then the top cover 6014 is separated from the protective casing 6012.
Specifically, the pump body shell 602 includes a wear-resistant layer 6021, a corrosion-resistant layer 6022 fixedly bonded to an outer surface of the wear-resistant layer 6021, and a high-temperature-resistant layer 6023 fixedly bonded to an outer surface of the corrosion-resistant layer 6022.
In this embodiment, the pump body case 602 is composed of three structural layers, namely, the wear-resistant layer 6021, the corrosion-resistant layer 6022, and the high-temperature-resistant layer 6023, so that the pump body case 602 can be better suitable for use in a high-corrosion environment.
Specifically, the wear-resistant layer 6021 is made of an ultra-high molecular weight polyethylene material, the corrosion-resistant layer 6022 is made of a polytetrafluoroethylene material, and the high-temperature-resistant layer 6023 is made of a polyurethane material.
In the embodiment, the ultra-high molecular weight polyethylene has strong wear resistance, the polytetrafluoroethylene material has strong corrosion resistance, and the polyurethane material has high-temperature resistance.
Specifically, one end of the spring 608 is fixedly connected with the inner side wall of the strip-shaped groove 606, and the other end of the spring 608 is fixedly connected with one side surface of the moving block 609.
In this embodiment, two ends of the spring 608 are respectively and fixedly connected to the inner side wall of the strip-shaped groove 606 and the surface of one side of the moving block 609, so that the connection performance is achieved and the corresponding buffering capacity is provided.
Specifically, one end of the limiting insertion rod 6010 is inserted into the inner wall of the limiting insertion hole 605, and the opening diameter of the limiting insertion hole 605 is matched with the design diameter of one end of the limiting insertion rod 6010.
In this embodiment, when the limiting insertion hole 605 is opened, the opening operation needs to be performed according to the design diameter of one end of the limiting insertion rod 6010, so that the one end of the limiting insertion rod 6010 is inserted into the inner wall of the limiting insertion hole 605 more stably.
Example 3:
the polyurethane resin is different from the embodiment 2 in that the high-peel hydrolysis-resistant polyurethane resin is prepared from the following raw materials in parts by weight: poly (1, 6-hexanediol adipate) glycol: 25 parts of polytetrahydrofuran diol PTMEG-3000: 27 parts of polyethylene glycol: 70 parts of trimethylolpropane: 8.5 parts of 4,4' -diphenylmethane diisocyanate: 12 parts of xylylene diisocyanate: 6.5 parts of organic bismuth catalyst: 0.35 part, isophorone diamine: 4.5 parts, KH-560: 3.5 parts of organosilicon antisticking agent: 0.8 part; the molecular weight of the poly adipic acid 1, 6-hexanediol glycol ester diol is 1500-2000; the molecular weight of the polyethylene glycol is 2000-2500; the mixture of the organosilicon antisticking agent AC-1800K and the antisticking agent FY-5080K is prepared from the following components in a mass ratio of 1: 0.88.
in this embodiment, the preparation method of the high-peel hydrolysis-resistant polyurethane resin adopts polyurethane production equipment to perform continuous production and preparation, and includes the following steps:
1) weighing the raw materials of the aliphatic non-yellowing polyurethane resin according to the parts by weight;
2) putting poly adipic acid 1, 6-hexanediol glycol, polytetrahydrofuran diol PTMEG-3000, polyethylene glycol, trimethylolpropane, 1/2 4,4' -diphenylmethane diisocyanate and 1/2 xylylene diisocyanate into a mixing and stirring kettle (1), and uniformly mixing to obtain a mixture;
3) conveying the mixture into a prepolymer tubular reactor (3) by using a feeding device (2), performing prepolymerization, controlling the temperature in the prepolymer tubular reactor (3) to be 70 ℃, and controlling the retention time of the mixture in the prepolymer tubular reactor (3) to be 20 min;
4) then continuously conveying the mixture into a reaction kettle (4) through a high-viscosity pump (6), controlling the temperature in the reaction kettle (4) to be 86 ℃, respectively adding the rest 4,4' -diphenylmethane diisocyanate, the rest xylylene diisocyanate and an organic bismuth catalyst, and reacting until the measured value of the NCO value is 0.35 percent after the addition is finished;
5) respectively adding isophorone diamine and KH-560 into the reaction kettle (4), controlling the temperature in the reaction kettle (4) to be 78 ℃ after the addition is finished, and carrying out heat preservation reaction for 3 hours;
6) stopping heating, adding the organic silicon anti-sticking agent, continuously stirring for 20min, and discharging to obtain the high-stripping hydrolysis-resistant polyurethane resin;
the whole reaction process in the reaction kettle (4) is in a nitrogen atmosphere, and a nitrogen charging device (5) is adopted to charge nitrogen into the reaction kettle (4).
The rest is the same as in example 2.
Example 4:
the polyurethane resin is different from the embodiment 2 in that the high-peel hydrolysis-resistant polyurethane resin is prepared from the following raw materials in parts by weight: poly (1, 6-hexanediol adipate) glycol: 20 parts of polytetrahydrofuran diol PTMEG-3000: 23.5 parts of polyethylene glycol: 60 parts of trimethylolpropane: 7 parts of 4,4' -diphenylmethane diisocyanate: 11 parts of xylylene diisocyanate: 5.8 parts of organic bismuth catalyst: 0.27 part of isophorone diamine: 4 parts, KH-560: 3 parts of organosilicon anti-sticking agent: 0.65 part; the molecular weight of the poly adipic acid 1, 6-hexanediol glycol ester diol is 1500-2000; the molecular weight of the polyethylene glycol is 2000-2500; the mixture of the organosilicon antisticking agent AC-1800K and the antisticking agent FY-5080K is prepared from the following components in a mass ratio of 1: 0.81.
in this embodiment, the preparation method of the high-peel hydrolysis-resistant polyurethane resin adopts polyurethane production equipment to perform continuous production and preparation, and includes the following steps:
1) weighing the raw materials of the aliphatic non-yellowing polyurethane resin according to the parts by weight;
2) putting poly adipic acid 1, 6-hexanediol glycol, polytetrahydrofuran diol PTMEG-3000, polyethylene glycol, trimethylolpropane, 1/2 4,4' -diphenylmethane diisocyanate and 1/2 xylylene diisocyanate into a mixing and stirring kettle (1), and uniformly mixing to obtain a mixture;
3) conveying the mixture into a prepolymer tubular reactor (3) by using a feeding device (2), carrying out prepolymerization, controlling the temperature in the prepolymer tubular reactor (3) to be 68 ℃, and controlling the retention time of the mixture in the prepolymer tubular reactor (3) to be 25 min;
4) then continuously conveying the mixture into a reaction kettle (4) through a high-viscosity pump (6), controlling the temperature in the reaction kettle (4) to be 85 ℃, respectively adding the rest 4,4' -diphenylmethane diisocyanate, the rest xylylene diisocyanate and an organic bismuth catalyst, and reacting until the measured value of the NCO value is 0.37 percent after the addition is finished;
5) respectively adding isophorone diamine and KH-560 into the reaction kettle (4), controlling the temperature in the reaction kettle (4) to be 77 ℃ after the addition is finished, and carrying out heat preservation reaction for 3.5 hours;
6) stopping heating, adding the organic silicon anti-sticking agent, continuously stirring for 30min, and discharging to obtain the high-stripping hydrolysis-resistant polyurethane resin;
the whole reaction process in the reaction kettle (4) is in a nitrogen atmosphere, and a nitrogen charging device (5) is adopted to charge nitrogen into the reaction kettle (4).
The rest is the same as in example 2.
The high peel hydrolysis resistant urethane resins obtained in examples 2 to 4 of the present invention were subjected to the following performance tests, and the test results are shown in table 1:
the high-peel hydrolysis-resistant polyurethane resins obtained in examples 2 to 4 of the present invention were respectively bonded to a base fabric (PET nonwoven fabric) to obtain polyurethane synthetic leather.
And testing the initial peel strength, curing the prepared polyurethane synthetic leather at 70 ℃ for 24h, testing the permanent peel strength, and testing the 5-week peel strength retention rate (70 ℃ multiplied by 95% humidity).
Hydrolysis resistance (peel strength versus original peel retention): the polyurethane synthetic leather prepared by using the high-peel hydrolysis-resistant polyurethane resin of the invention of the embodiment 2 to the embodiment 4 was cut into two pieces, one piece was tested for original peel strength (permanent peel strength), the other piece was immersed in a 10% sodium hydroxide aqueous solution at 25 ℃ for 12 hours, and then taken out, the residual sodium hydroxide solution was washed off, dried, and the hydrolyzed peel strength (permanent peel strength) was tested.
TABLE 1
The working principle and/or the using flow of the polyurethane production equipment adopted by the invention are as follows:
a polyurethane production device comprises a mixing and stirring kettle 1 for mixing (partial/total) raw materials for polyurethane production, and a feeding device 2 for feeding (partial/total) raw materials for polyurethane production, or called charging; in the actual use process, a plurality of feeding devices 2 can be arranged as necessary, and different raw materials can be added according to the needs, which can be understood by those skilled in the art. The prepolymer tubular reactor 3 is used for pre-polymerizing (partial/total) raw materials for producing polyurethane, the heating reaction kettle 4 is used for main reactions such as polymerization reaction, broad chain and the like of polyurethane, a polyurethane product is obtained by discharging, the nitrogen filling device 5, the high viscosity pump 6 is used for circulating and pressurizing high-viscosity liquid or solid-liquid mixture, and the finished product tank 7 is used for storing the polyurethane product discharged from the heating reaction kettle 4;
the mixing and stirring kettle 1, the feeding device 2, the prepolymer tubular reactor 3, the heating reaction kettle 4 and the finished product tank 7 are communicated in sequence through pipelines; a high-viscosity pump 6 is arranged on a pipeline between the prepolymer tubular reactor 3 and the heating reaction kettle 4 and a pipeline between the heating reaction kettle 4 and the finished product tank 7; the heating reaction kettle 4 is communicated with a nitrogen charging device 5; the nitrogen charging device 5 charges nitrogen into the heating reaction kettle 4 to ensure that the heating reaction kettle 4 is in nitrogen atmosphere when needed (in the projection process).
When using mixed stirred tank 1, at first open servo motor 104, servo motor 104 can drive the rotary rod 105 rotatory, rotary rod 105 can drive main shaft 108 rotation through square locating piece 1015 and square constant head tank 1016, main shaft 108 can drive the rotation of the first helical gear 1011 of a plurality of, first helical gear 1011 can drive second helical gear 1012 simultaneously and rotate, second helical gear 1012 can drive puddler 109 and rotate on fixed position, puddler 109 can drive stirring leaf 1010 and rotate, thereby make the inside liquid of a plurality of stirring leaf 1010 to the cauldron body 101 stir, moreover, the steam generator is simple in structure, can make the stirring, make its reaction abundant, thereby improve the quality of polyurethane production.
When the feeding device 2 is used, when the stirring barrel is high, the crank 208 is rotated to rotate the bidirectional threaded rod 203, the bidirectional threaded rod 203 rotates to drive the two threaded blocks 204 to be close to each other, the angles of the two rotating rods 205 are changed, and the lifting plate 206 is lifted. And through putting into the feed pipe 2013 and taking out the material in the raw materials, when the raw materials passes through discharging pipe 2014, go out water through water pump 2018 and carry out hydrologic cycle and cool down the raw materials to through semiconductor refrigeration piece 2019 further reduced the inside temperature of liquid storage tank 2017, make the cooling effect too better, in order to avoid material temperature high temperature, influence the raw materials chemical property condition to take place.
When the prepolymer tubular reactor 3 is used, a first material receiving pipe 302 and a second material receiving pipe 303 on a pipe body 301 are respectively added into a water supply device and a vacuum dehydrator, a material inlet 3013 is connected with a material supply device, a material outlet 3016 is connected with a neutralization kettle, materials entering the pipe body 301 sequentially pass through a coarse dredging net 308 and a fine dredging net 309 under the drive of a material pump 305, so that the materials are sequentially filtered to avoid the blockage of the materials in the pipe body 301, then a first electromagnetic valve 307 is opened to enable the materials in the pipe body 301 to flow into a return pipe 306, a fourth electromagnetic valve 3017 on the material inlet 3013 is opened to enable the mixed materials to be conveyed into the return pipe 306, meanwhile, a stirring impeller 3012 is driven by a drive motor 3011 to rotate to mix the mixed materials with the materials, then a second electromagnetic valve 3010 is opened to enable the mixed materials to flow back into the pipe body 301, so that the mixed materials can be fully mixed through the circular flow, in the process, heating pad 304 supplies heat to whole mixing and reaction process to in promote the speed of mixing and reacting, treat that the reaction finishes, close first solenoid valve 307 and open third solenoid valve 3014 and make the material in the body 301 get into in the storage tank 3015, so that carry out later manufacturing procedure, have certain practicality.
When the heating reaction kettle 4 is used, the electric heating plate 402 is electrified, after the electric heating plate 402 heats, the heat exchange medium in the inner cavity of the heat exchange barrel 403 is heated, at this time, if the reaction vessel 408 is positioned at the top end of the inner cavity of the heat exchange barrel 403, the heat exchange medium indirectly heats the reaction vessel 408, if the electric support rod 405 retracts, the reaction vessel 408 is driven to descend to the top surface of the electric heating plate 402, and at this time, the electric heating plate 402 directly heats the reaction vessel 408; the indirect heating has the advantages of stable temperature, suitability for long-term heating during reaction, rapid direct heating and suitability for the initial stage of reaction, and when the direct heating reaches the set temperature, the electric support rod 405 can push the reaction container 408 to rise for indirect heating; when the polyurethane raw material in the reaction vessel 408 reaches the set temperature, the electric support rod 405 continues to extend forward to push the protruding annular cover 404, at this time, the motor 4010 is started, the motor 4010 is engaged with the overturning gear 409 through the driving pinion 4011, and then the annular cross arm 407 drives the reaction vessel 408 to overturn, so that the polyurethane raw material or the finished product in the reaction vessel 408 is poured out.
When the nitrogen charging device 5 is used, nitrogen is conveyed to the space between the partition plates 502 through the first connecting pipe 504 and the second connecting pipe 505 by the nitrogen storage bottle 503, then the nitrogen is conveyed to the reaction kettle through the air outlet pipe 5020 for use, when the nitrogen charging device is used, the nitrogen which is different from the upper nitrogen to the lower nitrogen is conveyed, so that the nitrogen can be continuously conveyed when part of the nitrogen storage bottle 503 needs to be replaced, when the nitrogen storage bottle 503 is replaced, the insertion rod 5010 is separated from the connecting ring 506 by pulling the handle 5022, so that the dismounting effect is achieved, when the nitrogen charging device is installed, the insertion rod 5010 is reinserted into the connecting ring 506 through the resilience force of the supporting spring 508, so that the fixing effect is achieved, and when the device main body 501 is installed.
Claims (10)
1. The high-peel hydrolysis-resistant polyurethane resin is characterized by being prepared from the following raw materials in parts by weight:
poly (1, 6-hexanediol adipate) glycol: 15 to 25 parts of,
Polytetrahydrofuran diol PTMEG-3000: 20 to 27 parts of,
Polyethylene glycol: 50 to 70 parts of,
Trimethylolpropane: 5.5 to 8.5 parts of,
4,4' -diphenylmethane diisocyanate: 10 to 12 parts of,
Xylylene diisocyanate: 5 to 6.5 parts of,
Organic bismuth catalyst: 0.2 to 0.35 part,
Isophorone diamine: 3.5 to 4.5 parts of,
KH-560: 2.5 to 3.5 parts of,
Silicone anti-tack agent: 0.5-0.8 part;
the molecular weight of the poly adipic acid 1, 6-hexanediol glycol ester diol is 1500-2000;
the molecular weight of the polyethylene glycol is 2000-2500;
the mixture of the organosilicon antisticking agent AC-1800K and the antisticking agent FY-5080K is prepared from the following components in a mass ratio of 1: 0.75 to 0.88.
2. The method for preparing the high-peel hydrolysis-resistant polyurethane resin according to claim 1, wherein the polyurethane production equipment is used for continuous production and preparation, and the method comprises the following steps:
1) weighing the raw materials of the aliphatic non-yellowing polyurethane resin according to the parts by weight;
2) putting poly adipic acid 1, 6-hexanediol glycol, polytetrahydrofuran diol PTMEG-3000, polyethylene glycol, trimethylolpropane, 1/2 4,4' -diphenylmethane diisocyanate and 1/2 xylylene diisocyanate into a mixing and stirring kettle (1), and uniformly mixing to obtain a mixture;
3) conveying the mixture into a prepolymer tubular reactor (3) by using a feeding device (2), and carrying out prepolymerization, wherein the temperature in the prepolymer tubular reactor (3) is controlled to be 68 +/-2 ℃, and the retention time of the mixture in the prepolymer tubular reactor (3) is controlled to be 20-30 min;
4) then continuously conveying the mixture into a reaction kettle (4) through a high-viscosity pump (6), controlling the temperature in the reaction kettle (4) to be 84-86 ℃, respectively adding the rest 4,4' -diphenylmethane diisocyanate, the rest xylylene diisocyanate and an organic bismuth catalyst, and reacting until the measured value of NCO value is 0.35-0.40% after the addition is finished;
5) respectively adding isophorone diamine and KH-560 into the reaction kettle (4), controlling the temperature in the reaction kettle (4) to be 76-78 ℃ after the addition is finished, and carrying out heat preservation reaction for 3-4 h;
6) stopping heating, adding the organic silicon anti-sticking agent, continuously stirring for 20-40 min, and discharging to obtain the high-stripping hydrolysis-resistant polyurethane resin;
the whole reaction process in the reaction kettle (4) is in a nitrogen atmosphere, and a nitrogen charging device (5) is adopted to charge nitrogen into the reaction kettle (4).
3. The method for preparing a high-peel hydrolysis-resistant polyurethane resin according to claim 2, wherein: a polyurethane production facility which characterized in that: comprises a mixing and stirring kettle (1), a feeding device (2), a prepolymer tubular reactor (3), a heating reaction kettle (4), a nitrogen filling device (5), a high viscosity pump (6) and a finished product tank (7);
the mixing and stirring kettle (1), the feeding device (2), the prepolymer tubular reactor (3), the heating reaction kettle (4) and the finished product tank (7) are communicated in sequence through pipelines;
a high-viscosity pump (6) is arranged on a pipeline between the prepolymer tubular reactor (3) and the heating reaction kettle (4) and a pipeline between the heating reaction kettle (4) and the finished product tank (7);
the heating reaction kettle (4) is communicated with a nitrogen charging device (5).
4. The method for preparing a high-peel hydrolysis-resistant polyurethane resin according to claim 3, wherein: mix stirred tank (1) including the cauldron body (101), inner wall fixedly connected with mount (107) of the cauldron body (101), and mount (107) are two that are parallel to each other, two the common fixedly connected with fixed pipe (106) in one side that mount (107) are relative, the inside central point of the cauldron body (101) puts fixedly connected with A-frame (1017), the top of A-frame (1017) is rotated and is connected with main shaft (108), it is connected with puddler (109) to rotate jointly between fixed pipe (106) and the cauldron body (101), and puddler (109) are four, four of mutual symmetry the equal fixedly connected with stirring leaf (1010) in surface of puddler (109), the one end fixedly connected with second helical gear (1012) of puddler (109), and second helical gear (1012) are located the inside of fixed pipe (106), the position fixedly connected with first helical gear (1012) that the surface of main shaft (108) corresponds second helical gear (1012), the position fixedly connected with of helical gear (1012) is first 1011) The first bevel gear (1011) is meshed and connected with the second bevel gear (1012), one end, far away from the triangular support (1017), of the main shaft (108) is fixedly connected with a square positioning block (1015), the top of the kettle body (101) is provided with a kettle cover (102), the center of the top of the kettle cover (102) is fixedly connected with a servo motor (104), an output shaft of the servo motor (104) is fixedly connected with a rotating rod (105), and the rotating rod (105) is in through connection with the kettle cover (102);
the feeding device (2) comprises a base (201), a first groove (202) is formed in the upper surface of the base (201), a bidirectional threaded rod (203) is rotatably connected to the inside of the first groove (202), two thread blocks (204) are sleeved on the outer surface of the bidirectional threaded rod (203), the top ends of the two thread blocks (204) are rotatably connected with two rotating rods (205), the middle positions of the two rotating rods (205) are in crossed rotary connection, two lifting plates (206) are arranged above the two rotating rods (205), a second groove (209) is formed in the lower surface of each lifting plate (206), a fixing rod (2010) is fixedly connected to the inside of each second groove (209), two sliding sleeves (2011) are sleeved on the outer surface of each fixing rod (2010), and one ends, far away from the two thread blocks (204), of the two rotating rods (205) are respectively rotatably connected with the bottom ends of the two sliding sleeves (2011), the upper surface of lifter plate (206) is fixedly connected with charge pump (2012), fixed case (2015) and liquid reserve tank (2017) respectively, the material end union coupling that inhales of charge pump (2012) has inlet pipe (2013), the discharge end union coupling of charge pump (2012) has discharging pipe (2014), the one end that last charge pump (2012) was kept away from to discharging pipe (2014) extends to the inside of fixed case (2015) and stretches out from the roof of fixed case (2015), the top of liquid reserve tank (2017) is fixed to be inlayed and is linked with semiconductor refrigeration piece (2019), the hot junction fixedly connected with fin (2020) of semiconductor refrigeration piece (2019), the cold junction fixedly connected with of semiconductor refrigeration piece (2019) leads cold fin (2022), the inner wall fixedly connected with water pump (2018) of liquid reserve tank (2017), the play water end union coupling of water pump (2018) has cold water pipe (2016), the one end that water pump (2018) was kept away from to water pipe (2016) extends to fixed case (2018) inside spiral winding, discharge case (2017) inside The outer surface of the pipe (2014), and one end of the cold water pipe (2016), which is far away from the water pump (2018), is communicated with the side wall of the liquid storage tank (2017);
the prepolymer tubular reactor (3) comprises a pipe body (301), a first material receiving pipe (302) and a second material receiving pipe (303) are respectively arranged on two sides of the top end of the pipe body (301), a material pump (305) is fixedly connected to the outer side wall of the pipe body (301), a return pipe (306) is fixedly connected to the bottom end of the pipe body (301), a first electromagnetic valve (307) is arranged on one side, close to the pipe body (301), of the return pipe (306), a driving motor (3011) is fixedly connected to one side of the bottom end of the return pipe (306), an output shaft of the driving motor (3011) penetrates through the outer side wall of the return pipe (306) and extends to the inner side and is fixedly connected with a stirring impeller (3012), the top end of the return pipe (306) is fixedly connected with the top of the pipe body (301), and a second electromagnetic valve (3010) is arranged on the, the heating pad (304) is nested on the outer side walls of the return pipe (306) and the pipe body (301), a material storage tank (3015) is fixedly connected to one side, close to the return pipe (306), of the bottom end of the pipe body (301), and a third electromagnetic valve (3014) is arranged on one side, close to the material storage tank (3015), of the bottom end of the pipe body (301);
the heating reaction kettle (4) comprises a bottom plate (401) and a reaction container (408); the middle part fixed mounting of bottom plate (401) top surface has electric heating plate (402), the top fixedly connected with heat exchange bucket (403) of electric heating plate (402), the heater block of electric heating plate (402) runs through bottom surface to its inner chamber bottom of heat exchange bucket (403), the inner chamber of heat exchange bucket (403) is filled with heat exchange medium, the top surface fixedly connected with annular lid (404) of heat exchange bucket (403), the equal fixedly connected with electric support rod (405) in four corners of bottom plate (401) top surface, two homonymies the equal fixedly connected with in top of electric support rod (405) supports horizontal pole (406), two the middle part of supporting horizontal pole (406) is rotated and is connected with annular xarm (407), the middle part gomphosis of annular xarm (407) is fixed the outer wall of reaction vessel (408), the bottom of reaction vessel (408) runs through the centre bore of annular lid (404) to the inner chamber of heat exchange bucket (403) and intermittent type contact electric heating plate (403) 402) One end of the annular cross arm (407) is fixedly connected with a turnover gear (409), one side of the support cross rod (406) is fixedly connected with an electric motor (4010), an output shaft of the electric motor (4010) is fixedly connected with a driving pinion (4011), and the driving pinion (4011) is meshed with the turnover gear (409);
the nitrogen charging device (5) comprises a device body (501); the inner side wall of the device body (501) is fixedly connected with a partition board (502), the inner bottom wall of the device body (501) is provided with a nitrogen storage bottle (503), the bottom of the partition board (502) is fixedly connected with a first connecting pipe (504), the end of the nitrogen storage bottle (503) is fixedly connected with a second connecting pipe (505), the surfaces of the first connecting pipe (504) and the second connecting pipe (505) are fixedly connected with a connecting ring (506), the surface of the second connecting pipe (505) is fixedly connected with a supporting plate (507), the top of the supporting plate (507) is fixedly connected with a supporting spring (508), the top of the supporting spring (508) is fixedly connected with a connecting rod (509), the bottom of the connecting rod (509) is fixedly connected with an insert rod (5010), the insert rod (5010) is in through connection with the connecting ring (506), and the bottom of the device body (501) is fixedly connected with a base (, a special-shaped groove (5012) is formed in the top of the base (5011), a special-shaped plate (5013) is fixedly connected to the bottom of the device body (501), and the special-shaped plate (5013) is in sliding connection with the inner wall of the special-shaped groove (5012);
the high-viscosity pump (6) comprises an electric motor (601), a pump body shell (602) and a mounting plate (603); the outer fixed surface of motor (601) is connected with connecting plate (604), spacing jack (605) have all been seted up on the both sides surface of connecting plate (604), bar groove (606) have been seted up to the upper end surface of motor (601), the inside fixedly connected with dead lever (607) of bar groove (606), the surface cover of dead lever (607) is equipped with spring (608), the surface sliding connection of dead lever (607) has movable block (609), one side fixedly connected with spacing inserted bar (6010) of movable block (609), the upper end surface of movable block (609) has been seted up and has been detained hole (6011), the upper end fixedly connected with protecting crust (6012) of mounting panel (603), the output fixed mounting of motor (601) has shaft coupling (6013).
5. The method for preparing a high-peel hydrolysis-resistant polyurethane resin according to claim 3, wherein: the center positions of the outer surfaces of the two fixing frames (107) are respectively provided with an opening (1014), the two fixing frames (107) are communicated with a fixing pipe (106) through the openings (1014), and the spindle (108) is in penetrating connection with the fixing frames (107) and the fixing pipe (106);
a hexagonal nut (103) is arranged between the kettle body (101) and the kettle cover (102) together, and the kettle body (101) is fixedly connected with the kettle cover (102) through the hexagonal nut (103);
the outer surfaces of the two fixing frames (107) are provided with openings (1013);
the outer surface of one end of the rotating rod (105) is provided with a square positioning groove (1016), and the square positioning block (1015) is connected with the square positioning groove (1016) in an embedded manner;
the bottom of the kettle body (101) is provided with a discharge hole, and the top of the kettle cover (102) is provided with a feed hole.
6. The method for preparing a high-peel hydrolysis-resistant polyurethane resin according to claim 3, wherein: one end of the bidirectional threaded rod (203) penetrates through the side wall of the first groove (202) and extends to the outside of the base (201) to be fixedly connected with a crank (208);
the upper surface of the base (201) is fixedly connected with four guide rods (207), and the top ends of the four guide rods (207) penetrate through the side wall of the lifting plate (206) and extend to the outside;
the inside of the liquid storage tank (2017) is provided with circulating cold water;
the upper surface of the radiating fin (2020) is fixedly connected with a radiating fan (2021);
the cold guide fin (2022) extends to the inside of the liquid storage tank (2017).
7. The method for preparing a high-peel hydrolysis-resistant polyurethane resin according to claim 3, wherein: a feeding port (3013) is arranged at the position, close to the first electromagnetic valve (307), of the bottom end of the return pipe (306);
a discharge hole (3016) is formed in the bottom end of the material storage tank (3015);
the inner sides of the feeding port (3013) and the discharging port (3016) are provided with fourth electromagnetic valves (3017);
a coarse dredging net (308) is arranged on one side, close to the first material receiving pipe (302) and the second material receiving pipe (303), of the inner side wall of the pipe body (301), a fine dredging net (309) is arranged on one side, far away from the first material receiving pipe (302) and the second material receiving pipe (303), of the inner side wall of the pipe body (301), and the top end of the return pipe (306) is located on the top side of the coarse dredging net (308);
the material pump (305) is positioned at the middle side between the coarse dredging net (308) and the fine dredging net (309).
8. The method for preparing a high-peel hydrolysis-resistant polyurethane resin according to claim 3, wherein: an electric cabinet (4012) is fixedly mounted on one side of the base plate (401), an automatic temperature controller (4013), a motor driver (4014) and a power controller (4015) are fixedly mounted in the electric cabinet (4012), the automatic temperature controller (4013) is electrically connected with control ends of the motor driver (4014) and the power controller (4015), the motor driver (4014) is electrically connected with a motor (4010) and four electric support rods (405), and the power controller (4015) is electrically connected with an electric heating plate (402);
the inner bottom wall of the reaction container (408) is fixedly connected with a heat conduction column (4016), and the heat conduction column (4016) extends to the middle part of the inner cavity of the reaction container (408);
a first thermal sensor (4017) is fixedly connected to the inner cavity of the heat exchange barrel (403), a second thermal sensor (4018) is fixedly connected to the inner cavity of the reaction container (408), and the first thermal sensor (4017) and the second thermal sensor (4018) are both electrically connected with the signal end of the automatic temperature controller (4013);
the electric heating plate (402) is a resistor type or a capacitor type, and the reaction vessel (408) is made of stainless steel materials.
9. The method for preparing a high-peel hydrolysis-resistant polyurethane resin according to claim 3, wherein: a fixed plate (5014) is fixedly connected to the inner bottom wall of the device body (501), a clamping spring (5015) is fixedly connected to the side edge of the fixed plate (5014), a clamping plate (5016) is fixedly connected to the end portion of the clamping spring (5015), and the clamping plate (5016) is in contact with the nitrogen storage bottle (503);
a bolt (5017) is arranged at the top of the base (5011), a threaded hole (5018) is formed in the bottom of the special-shaped groove (5012), and the bolt (5017) penetrates through the special-shaped plate (5013) and is in threaded connection with the threaded hole (5018);
the surface of the device main body (501) is rotatably connected with a device door (5019) through a hinge, and the side edge of the device main body (501) is fixedly connected with an air outlet pipe (5020);
the top of the supporting plate (507) is fixedly connected with a guide rod (5021), and the guide rod (5021) is in through connection with a connecting rod (509);
the top of the connecting rod (509) is fixedly connected with a handle (5022), and the surface of the first connecting pipe (504) is provided with an electromagnetic valve.
10. The method for preparing a high-peel hydrolysis-resistant polyurethane resin according to claim 3, wherein: a top cover (6014) is arranged at the upper end of the protective shell (6012), a fastening screw (6015) is in threaded connection with the upper end of the top cover (6014), a threaded hole (6016) is formed in the upper end of the protective shell (6012), and an elastic rubber block (6017) is fixedly connected to the lower end of the mounting plate (603);
the pump body shell (602) comprises a wear-resistant layer (60201), wherein a corrosion-resistant layer (60202) is fixedly bonded to the outer surface of the wear-resistant layer (60201), and a high-temperature-resistant layer (60203) is fixedly bonded to the outer surface of the corrosion-resistant layer (60202);
the wear-resistant layer (60201) is made of an ultra-high molecular weight polyethylene material, the corrosion-resistant layer (60202) is made of a polytetrafluoroethylene material, and the high-temperature-resistant layer (60203) is made of a polyurethane material;
one end of the spring (608) is fixedly connected with the inner side wall of the strip-shaped groove (606), and the other end of the spring (608) is fixedly connected with the surface of one side of the moving block (609);
one end of the limiting insertion rod (6010) is inserted into the inner wall of the limiting insertion hole (605), and the opening diameter of the limiting insertion hole (605) is matched with the design diameter of one end of the limiting insertion rod (6010).
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CN110835401A (en) * | 2019-09-24 | 2020-02-25 | 浙江禾欣科技有限公司 | Waterborne polyurethane surface layer resin and preparation method thereof |
CN110951033A (en) * | 2019-12-19 | 2020-04-03 | 超然(福建)新材料科技有限公司 | Hydrolysis-resistant polyurethane resin and preparation method thereof |
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CN101381449A (en) * | 2008-10-14 | 2009-03-11 | 太仓市旭川树脂有限公司 | Polyurethane resin for artificial leather |
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