Process and device for preparing low-VOC polyurethane raw material

By mixing low-VOC polyester polyols with polyurethane prepolymers and other additives under nitrogen protection, low-VOC polyurethane raw materials are generated, solving the problem of high VOC content in existing technologies and realizing the preparation of environmentally friendly, healthy and safe polyurethane raw materials suitable for industrial production.

WO2026000857A1PCT designated stage Publication Date: 2026-01-02JIANGSU HENGGUANG NEW MATERIAL CO LTD
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Patent Information

Application Number
PCT/CN2024/138797
Authority / Receiving Office
WO · WO
Patent Type
Applications
Current Assignee / Owner
Priority Date
2024-06-24
Filing Date
2024-12-12
Publication Date
2026-01-02

AI Technical Summary

Technical Problem

Existing polyurethane raw materials contain high levels of VOCs, which cannot meet increasingly stringent environmental protection requirements.

Method used

Polyester polyols at concentrations below 100 ppm are mixed with polyurethane prepolymers, and flame retardants, stabilizers, organotin catalysts, silicone defoamers, and calcium carbonate are added under nitrogen protection. The mixture is then heated to produce a low-VOC polyurethane raw material.

Benefits of technology

Low-VOC polyurethane raw materials that meet environmental protection, health, and safety requirements have been prepared, exhibiting high production efficiency and excellent performance, and are suitable for industrial production.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present invention relates to the technical field of chemical preparation, and in particular to a process and device for preparing a low-VOC polyurethane raw material. The process comprises: preparing a polyurethane prepolymer; adding a polyester polyol having a VOC content of less than 100 ppm and the polyurethane prepolymer to a preparation device for mixing; continuing to add a flame retardant, a stabilizer, an organotin catalyst, a silicone defoamer, and calcium carbonate to the preparation device for uniform mixing; and introducing nitrogen into the preparation device for protection and then heating the mixture for a reaction to generate the low-VOC polyurethane raw material. In order to prevent the mixture from being oxidized in the reaction process, nitrogen is introduced for protection. Subsequently, the mixture is heated to promote the reaction between the components, ultimately resulting in the low-VOC polyurethane raw material. By means of these steps, the low-VOC polyurethane raw material that meets environmental friendliness, health, and safety requirements can be prepared. The preparation process not only has relatively high production efficiency, but can also ensure the excellent performance of the obtained product, and is suitable for industrial production.
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Description

Preparation process and device of low VOC polyurethane raw material TECHNICAL FIELD

[0001] The present application relates to the technical field of chemical preparation, and particularly relates to a preparation process and device of low VOC polyurethane raw material. BACKGROUND

[0002] VOC polyurethane is a polymer material with high molecular weight, which is formed by the reaction of isocyanate and polyol. It has excellent wear resistance, weather resistance, chemical resistance and adhesion, and is widely used in the fields of coatings, foams, adhesives and elastomers. VOC polyurethane has high reactivity, can be quickly cured at room temperature, and can be used in various construction methods, such as spraying, brushing, pouring, etc.

[0003] The existing polyurethane raw material contains high VOC, which cannot meet the increasingly stringent environmental protection requirements. SUMMARY

[0004] The present application aims to provide a preparation process and device of low VOC polyurethane raw material, which can have high production efficiency, and can ensure the excellent performance of the obtained product, and is suitable for industrial production.

[0005] To achieve the above-mentioned purpose, in the first aspect, the present application further provides a preparation process of low VOC polyurethane raw material, comprising: preparing polyurethane prepolymer;

[0006] The polyester polyol with VOC content lower than 100 ppm and the polyurethane prepolymer are added into the preparation device for mixing;

[0007] The flame retardant, the stabilizer, the organic tin catalyst, the silicone defoaming agent and the calcium carbonate are continuously added into the preparation device for mixing uniformly;

[0008] Nitrogen is introduced into the preparation device for protection, and then the mixture is heated to react to generate low VOC polyurethane raw material.

[0009] In a second aspect, the present application provides a device for preparing low VOC polyurethane raw materials, which comprises a supporting assembly, a feeding assembly, a mixing assembly and a nitrogen protection assembly, the supporting assembly comprises a base, a supporting frame, a mixing shell, a cover plate and a heater, the supporting frame is fixedly connected with the base and located at the top of the base, the mixing shell is fixedly connected with the supporting frame and located at one side of the mixing shell, the cover plate is arranged on the top of the mixing shell, and the heater is arranged outside the mixing shell, the feeding assembly is arranged on the cover plate and used for adding raw materials into the mixing shell, the mixing assembly comprises a stirring motor, a stirring rod and stirring blades, the stirring motor is fixed on the cover plate, the stirring rod is connected with the output end of the stirring motor, and the stirring blades are fixedly connected with the stirring rod and located in the mixing shell, and the nitrogen protection assembly comprises a driving cylinder, a sliding plate, a control valve, a connecting pipe, a sliding pipe, a gas pump and a nitrogen cylinder, the sliding plate is slidingly arranged below the cover plate, the output end of the driving cylinder is connected with the sliding plate, the control valve is fixed in an opening on the sliding plate, the connecting pipe is fixed on the cover plate, the sliding pipe is slidingly connected with the connecting pipe and located at one side of the connecting pipe, the gas pump is in communication with the connecting pipe, and the nitrogen cylinder is in communication with the gas pump.

[0010] The cover plate comprises a cover plate body, a plurality of clamping plates and a plurality of supporting springs, the plurality of clamping plates are rotatably connected with the cover plate body and located around the cover plate body, and the plurality of supporting springs are arranged at one side of the plurality of clamping plates respectively.

[0011] The cover plate further comprises a second sealing ring, the second sealing ring is fixedly connected with the cover plate body and located between the cover plate body and the mixing shell.

[0012] The supporting assembly further comprises a clamping structure, the clamping structure comprises a sliding block, a second spring and a triangular block, the sliding block is slidingly connected with the cover plate body and located at the inner side of the cover plate body, the second spring is arranged between the sliding block and the cover plate body, and the triangular block is fixed on the sliding block.

[0013] In a third aspect, the present application provides a low VOC polyurethane raw material, which is composed of the following components by weight: 50-95 parts of a polyurethane prepolymer, 5-20 parts of a polyester polyol with a VOC content of less than 100 ppm, 0.1-5 parts of a flame retardant, 0.1-5 parts of a stabilizer, 0.1-5 parts of an organic tin catalyst, 0.1-5 parts of a silicone defoaming agent and 1-5 parts of calcium carbonate.

[0014] The polyurethane prepolymer is prepared by the reaction of isocyanate and polyol.

[0015] wherein the flame retardant includes a phosphorus-based flame retardant and a halogen-based flame retardant.

[0016] The preparation process and device of the low-VOC polyurethane raw material of the present application comprises: preparing a polyurethane prepolymer; adding a polyester polyol with a VOC content of less than 100 ppm and the polyurethane prepolymer into a preparation device for mixing; continuously adding a flame retardant, a stabilizer, an organic tin catalyst, a silicone defoaming agent, and calcium carbonate into the preparation device for mixing uniformly; introducing nitrogen into the preparation device for protection, and then heating the mixture to make it react to generate the low-VOC polyurethane raw material. In order to prevent the mixture from being oxidized during the reaction, nitrogen is introduced for protection. Subsequently, the mixture is heated to promote the reaction between the components, and finally the low-VOC polyurethane raw material is generated. Through the above steps, the low-VOC polyurethane raw material meeting the requirements of environmental protection, health, and safety can be prepared. The preparation process not only has high production efficiency, but also can ensure the excellent performance of the obtained product, and is suitable for industrial production. BRIEF DESCRIPTION OF DRAWINGS

[0017] In order to more clearly illustrate the technical solutions of the embodiments of the present application or the prior art, the drawings needed to be used in the embodiments or prior art description will be briefly introduced below. Obviously, the drawings in the following description are only some embodiments of the present application, and other drawings can be obtained by those skilled in the art without creative labor on the basis of these drawings.

[0018] Fig. 1 is a flow chart of the preparation process of a low-VOC polyurethane raw material of the second embodiment of the present application.

[0019] Fig. 2 is a structural diagram of the preparation device of the third embodiment of the present application.

[0020] Fig. 3 is a transverse cross-sectional structural diagram of the preparation device of the third embodiment of the present application.

[0021] Fig. 4 is a partial enlarged view of detail A of Fig. 3.

[0022] Fig. 5 is a longitudinal cross-sectional structural diagram of the preparation device of the third embodiment of the present application.

[0023] Support assembly 301, feeding assembly 302, mixing assembly 303, nitrogen protection assembly 304, base 305, support frame 306, mixing shell 307, cover plate 308, heater 309, stirring motor 310, stirring rod 311, stirring blade 312, driving cylinder 313, sliding plate 314, control valve 315, connecting pipe 316, sliding pipe 317, air pump 318, nitrogen cylinder 319, cover plate body 320, clamping plate 321, support spring 322, second sealing ring 323, push ring 324, push cylinder 325, engagement structure 326, sliding block 327, second spring 328, triangular block 329, heating coil 330, heat preservation layer 331, feeder 332, feeding valve 333, flow meter 334. DETAILED DESCRIPTION

[0024] Embodiments of the present application are described in detail below with reference to examples illustrated in the accompanying drawings, in which the same or similar components are denoted by the same or similar reference numerals throughout. The embodiments described below by reference to the accompanying drawings are exemplary and are intended to explain the present application, and should not be construed as limiting the present application.

[0025] First embodiment

[0026] The present application provides a low VOC polyurethane raw material, which is composed of the following components by weight: 50-95 parts of polyurethane prepolymer; 5-20 parts of polyester polyol with VOC content less than 100 ppm; 0.1-5 parts of flame retardant; 0.1-5 parts of stabilizer; 0.1-5 parts of organic tin catalyst; 0.1-5 parts of silicone defoaming agent; 1-5 parts of calcium carbonate.

[0027] The polyurethane prepolymer is prepared by reacting isocyanate and polyol.

[0028] The flame retardant includes phosphorus-based flame retardant and halogen-based flame retardant.

[0029] In the embodiment, the low VOC polyurethane raw material is composed of the following components by weight: polyurethane prepolymer: 50-95 parts. The polyurethane prepolymer is prepared by the reaction of isocyanate and polyol, and has good bonding performance, mechanical performance and wear resistance. Polyester polyol with VOC content less than 100 ppm: 5-20 parts. Such polyester polyol has low volatility, can effectively reduce the VOC content of the polyurethane raw material, and meets the environmental protection requirements. Flame retardant: 0.1-5 parts. The flame retardant includes phosphorus-based flame retardant and halogen-based flame retardant, which can improve the fireproof performance of the polyurethane raw material and protect personal and property safety. Stabilizer: 0.1-5 parts. The stabilizer can improve the heat resistance, weather resistance and durability of the polyurethane raw material, and prolong the service life of the product. Organic tin catalyst: 0.1-5 parts. The organic tin catalyst can accelerate the curing reaction of the polyurethane raw material and improve the production efficiency. Silicone defoamer: 0.1-5 parts. The silicone defoamer can effectively eliminate the bubbles generated in the preparation and curing process of the polyurethane raw material, and improve the appearance quality of the product. Calcium carbonate: 1-5 parts. As a filler, calcium carbonate can improve the mechanical properties and wear resistance of the polyurethane raw material, while reducing the cost.

[0030] The low VOC polyurethane raw material of the present application has the advantages of low volatility, environmental protection, safety and the like while ensuring performance, meets the requirements of environmental protection and health in China, and has a wide application prospect.

[0031] Second embodiment

[0032] Referring to FIG. 1, on the basis of the first embodiment, the present application further provides a preparation process of the low VOC polyurethane raw material, comprising:

[0033] S101 preparing polyurethane prepolymer;

[0034] Firstly, suitable isocyanate and polyol are selected to prepare polyurethane prepolymer through polymerization reaction. The polyurethane prepolymer should have good physical and chemical properties to provide a good basis for subsequent reactions.

[0035] S102 adding polyester polyol with VOC content less than 100 ppm and polyurethane prepolymer into a preparation device for mixing;

[0036] The prepared polyurethane prepolymer and polyester polyol with VOC content less than 100 ppm are put into the preparation device, and the two are fully mixed by stirring or other methods to ensure uniformity.

[0037] S103 continuously adding flame retardant, stabilizer, organic tin catalyst, silicone defoamer and calcium carbonate into the preparation device for mixing evenly;

[0038] In the mixed polyurethane prepolymer and polyester polyol, gradually add flame retardant, stabilizer, organic tin catalyst, silicone defoaming agent and calcium carbonate, continue to stir until mixed evenly. This helps to improve the performance of low VOC polyurethane raw materials.

[0039] S104 in preparation device into nitrogen protection, and then heated mixture, so that the reaction of low VOC polyurethane raw materials.

[0040] In order to prevent the mixture from being oxidized during the reaction, nitrogen is introduced for protection. Subsequently, the mixture is heated to promote the reaction between the components, and finally the low VOC polyurethane raw material is obtained.

[0041] Through the above steps, low VOC polyurethane raw materials meeting the requirements of environmental protection, health and safety can be prepared. The preparation process not only has high production efficiency, but also can ensure the excellent performance of the obtained product, and is suitable for industrial production.

[0042] Third embodiment

[0043] Referring to FIGS. 2-5, on the basis of the second embodiment, the application further provides a preparation device of low VOC polyurethane raw materials, comprising a supporting assembly 301, a feeding assembly 302, a mixing assembly 303 and a nitrogen protection assembly 304, the supporting assembly 301 comprises a base 305, a supporting frame 306, a mixing shell 307, a cover plate 308 and a heater 309, the supporting frame 306 is fixedly connected with the base 305 and located at the top of the base 305, the mixing shell 307 is fixedly connected with the supporting frame 306 and located at one side of the mixing shell 307, the cover plate 308 is arranged at the top of the mixing shell 307, the heater 309 is arranged outside the mixing shell 307, the feeding assembly 302 is arranged on the cover plate 308 and used for adding raw materials into the mixing shell 307, the mixing assembly 303 comprises a stirring motor 310, a stirring rod 311 and stirring blades 312, the stirring motor 310 is fixed on the cover plate 308, the stirring rod 311 is connected with the output end of the stirring motor 310, the stirring blades 312 are fixedly connected with the stirring rod 311 and located in the mixing shell 307, the nitrogen protection assembly 304 comprises a driving cylinder 313, a sliding plate 314, a control valve 315, a connecting pipe 316, a sliding pipe 317, a gas pump 318 and a nitrogen cylinder 319, the sliding plate 314 is slidingly arranged below the cover plate 308, the output end of the driving cylinder 313 is connected with the sliding plate 314, the control valve 315 is fixed in an opening on the sliding plate 314, the connecting pipe 316 is fixed on the cover plate 308, the sliding pipe 317 is slidingly connected with the connecting pipe 316 and located at one side of the connecting pipe 316, the gas pump 318 is in communication with the connecting pipe 316, and the nitrogen cylinder 319 is in communication with the gas pump 318.

[0044] In the present embodiment, the support assembly 301 is the base of the preparation device system, providing stable physical support for the entire preparation device. The base 305 is the foundation of the support assembly 301, and the support frame 306 is connected to the base 305 and located on the top of the base 305 to provide support for other components. The mixing shell 307 is fixed on the support frame 306 and is used to contain raw materials and carry out mixing reactions. The cover plate 308 is arranged on the top of the mixing shell 307 and is used to seal and protect the mixture. The heater 309 is arranged on the outside of the mixing shell 307 to provide a suitable reaction temperature. The feeding assembly 302 is arranged on the cover plate 308 and is used to add raw materials to the mixing shell 307. The feeder 332 is used to feed raw materials into the preparation device, the feeding valve 333 controls the flow of raw materials, and the flow meter 334 monitors the flow of raw materials to ensure accurate control of the proportion of reactants. The stirring motor 310 is fixed on the cover plate 308 and is connected to the stirring blade 312 through the stirring rod 311, and the stirring blade 312 is located inside the mixing shell 307 and is used to stir the mixture. The design of the mixing assembly 303 should ensure the uniformity and stability of the mixture to improve the reaction efficiency and the quality of the product. The nitrogen protection assembly 304 is used to protect the mixture inside the preparation device from oxidation. Specifically, after the raw materials are added to the mixing shell 307, the driving cylinder 313 is started to drive the sliding plate 314 to move downward, at this time the control valve 315 is opened, so that air can enter the space above the sliding plate 314 from the control valve 315, then the control valve 315 is closed, then the air pump 318 is started, so that the nitrogen in the nitrogen cylinder 319 can enter the sliding pipe 317 through the connecting pipe 316, then enter the bottom of the sliding plate 314, at this time the control valve 315 is closed, so that the sliding plate 314 can be lifted up under the action of nitrogen, so that air can be quickly discharged through the exhaust valve, so that the inflation efficiency is higher, the exhaust gas is more comprehensive, and the quality of the production of VOC polyurethane raw materials is improved.

[0045] The cover plate 308 includes a cover plate body 320, a plurality of clamping plates 321, and a plurality of support springs 322. The plurality of clamping plates 321 are rotatably connected to the cover plate body 320 and are located around the cover plate body 320. The plurality of support springs 322 are arranged on one side of the plurality of clamping plates 321. In order to improve the sealing effect of the cover plate body 320, a plurality of clamping plates 321 are arranged on the cover plate body 320, so that the cover plate body 320 can be fixed with the mixing shell 307 through the plurality of clamping plates 321 supported by the support springs 322 when sealing, thereby improving the sealing effect.

[0046] The cover plate 308 also includes a second sealing ring 323, which is fixedly connected with the cover plate body 320 and located between the cover plate body 320 and the mixing shell 307. The sealing effect can be further enhanced by the second sealing ring 323.

[0047] The cover plate 308 also includes a push ring 324 and a push cylinder 325. The push ring 324 is slidingly arranged on the mixing shell 307 and close to the clamping plate 321. The output end of the push cylinder 325 is connected with the push ring 324. Starting the push cylinder 325 can drive the push ring 324 to move upward, thereby simultaneously pushing open and unlocking multiple clamping plates 321, making it more convenient to use.

[0048] The support assembly 301 also includes a clamping structure 326, which includes a sliding block 327, a second spring 328, and a triangular block 329. The sliding block 327 is slidingly connected with the cover plate body 320 and located on the inner side of the cover plate body 320. The second spring 328 is arranged between the sliding block 327 and the cover plate body 320. The triangular block 329 is fixed on the sliding block 327. When the sliding plate 314 moves to the top of the cover plate 308, the sliding plate 314 can be limited by the triangular block 329, thereby facilitating subsequent use. When the sliding plate 314 moves downward, the second spring 328 can be compressed, so that the sliding plate 314 can continue to move downward.

[0049] The heater 309 includes a heating coil 330 and a heat preservation layer 331. The heating coil 330 is arranged on the outer side of the mixing shell 307. The heat preservation layer 331 is arranged on the outer side of the heating coil 330. The heating coil 330 is arranged on the outer side of the mixing shell 307 to control the reaction temperature by heating. The heat preservation layer 331 is arranged on the outer side of the heating coil 330 to reduce heat loss and maintain stable reaction temperature. The design of the heater 309 should ensure temperature control and energy efficiency of the reaction.

[0050] The feeding assembly 302 includes a feeder 332, a feeding valve 333, and a flow meter 334. The feeding valve 333 is in communication with the cover plate body 320. The flow meter 334 is arranged on the feeding valve 333. The feeder 332 is arranged on the flow meter 334. The feeding valve 333 controls the flow of raw materials. The flow meter 334 monitors the flow of raw materials. The feeder 332 is arranged on the flow meter 334 to feed raw materials into the preparation device. The design of the feeding assembly 302 should ensure accurate metering and uniform distribution of raw materials to ensure uniformity of the reaction and quality of the product.

[0051] Through cooperation of the components, the low VOC polyurethane raw material preparation process can realize efficient and uniform mixing reaction, and ensure excellent performance of the obtained raw material.

[0052] The above only discloses a preferred embodiment of the present application, and of course cannot limit the scope of the present application, and those skilled in the art can understand that all or part of the above-mentioned processes are implemented, and equivalent changes are made according to the claims of the present application, which still belongs to the scope covered by the present application.

Claims

1. A preparation process for a low-VOC polyurethane raw material, Its features are, Includes: preparing polyurethane prepolymer; Polyester polyols with VOC content below 100 ppm and polyurethane prepolymers are added to the preparation device and mixed. Flame retardant, stabilizer, organotin catalyst, silicone defoamer and calcium carbonate are added to the preparation device and mixed evenly; Nitrogen gas is introduced into the preparation device for protection, and then the mixture is heated to react and generate low-VOC polyurethane raw material.

2. An apparatus for preparing a low-VOC polyurethane raw material, applied to the preparation process of a low-VOC polyurethane raw material as described in claim 1, characterized in that, The system includes a support assembly, a feeding assembly, a mixing assembly, and a nitrogen protection assembly. The support assembly includes a base, a support frame, a mixing shell, a cover plate, and a heater. The support frame is fixedly connected to the base and located on top of the base. The mixing shell is fixedly connected to the support frame and located on one side of the mixing shell. The cover plate is located on top of the mixing shell. The heater is located on the outside of the mixing shell. The feeding assembly is located on the cover plate and is used to add raw materials to the mixing shell. The mixing assembly includes a stirring motor, a stirring rod, and stirring blades. The stirring motor is fixed to the cover plate. The stirring rod is connected to the output end of the stirring motor, the stirring blade is fixedly connected to the stirring rod and located inside the mixing shell, the nitrogen protection assembly includes a drive cylinder, a sliding plate, a control valve, a connecting pipe, a sliding tube, an air pump and a nitrogen cylinder, the sliding plate is slidably disposed below the cover plate, the output end of the drive cylinder is connected to the sliding plate, the control valve is fixed in the opening of the sliding plate, the connecting pipe is fixed to the cover plate, the sliding tube is slidably connected to the connecting pipe and located on one side of the connecting pipe, the air pump is connected to the connecting pipe, and the nitrogen cylinder is connected to the air pump.

3. The apparatus for preparing low-VOC polyurethane raw materials as described in claim 2, characterized in that, The cover plate includes a cover plate body, multiple clamping plates, and multiple supporting springs. The multiple clamping plates are rotatably connected to the cover plate body and are located around the cover plate body. The multiple supporting springs are respectively disposed on one side of the multiple clamping plates.

4. The apparatus for preparing low-VOC polyurethane raw materials as described in claim 3, characterized in that, The cover plate also includes a second sealing ring, which is fixedly connected to the cover plate body and located between the cover plate body and the mixing shell.

5. The apparatus for preparing low-VOC polyurethane raw materials as described in claim 4, characterized in that, The support assembly further includes a locking structure, which includes a slider, a second spring, and a triangular block. The slider is slidably connected to the cover plate body and is located inside the cover plate body. The second spring is disposed between the slider and the cover plate body, and the triangular block is fixed on the slider.

6. A low-VOC polyurethane raw material, characterized in that, The low-VOC polyurethane raw material is composed of the following components in parts by weight: 50-95 parts of polyurethane prepolymer; 5-20 parts of polyester polyol with a VOC content of less than 100 ppm; 0.1-5 parts of flame retardant; 0.1-5 parts of stabilizer; 0.1-5 parts of organotin catalyst; 0.1-5 parts of silicone defoamer; and 1-5 parts of calcium carbonate.

7. The low-VOC polyurethane raw material as described in claim 6, characterized in that, The polyurethane prepolymer is prepared by reacting isocyanate and polyol.

8. The low-VOC polyurethane raw material as described in claim 7, characterized in that, Flame retardants include phosphorus-based flame retardants and halogen-based flame retardants.

Citation Information

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