CN217313359U - Waterborne polyurethane dispersion apparatus for producing - Google Patents

Waterborne polyurethane dispersion apparatus for producing Download PDF

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Publication number
CN217313359U
CN217313359U CN202220527199.3U CN202220527199U CN217313359U CN 217313359 U CN217313359 U CN 217313359U CN 202220527199 U CN202220527199 U CN 202220527199U CN 217313359 U CN217313359 U CN 217313359U
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kettle
metering tank
pipeline
dispersion
polymerization reaction
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张闯
路玲
孟召磊
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Shandong Century United New Material Technology Co ltd
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Shandong Century United New Material Technology Co ltd
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Abstract

The utility model relates to an aqueous polyurethane production technical field, concretely relates to aqueous polyurethane dispersion apparatus for producing. The production device of the aqueous polyurethane dispersion comprises a polymerization reaction kettle, a high-speed dispersion kettle and a desolventizing kettle which are sequentially connected, wherein a feed inlet of the polymerization reaction kettle is connected with a monomer metering tank and an auxiliary agent metering tank, and discharge outlets of the monomer metering tank and the auxiliary agent metering tank are connected with a nitrogen purging pipeline; the top of the polymerization reaction kettle is provided with a condenser and an exhaust pipeline, and a discharge port is connected with a feed port of the high-speed dispersion kettle; two groups of dispersion discs and a group of stirrers are arranged in the high-speed dispersion kettle; the discharge hole of the high-speed dispersion kettle is connected with the feed inlet of the desolventizing kettle; the bottom of the desolventizing kettle is connected with a product output pipeline, and a top gas phase outlet is connected with a solvent recovery tank after passing through a cooler. The utility model discloses a polymerization kettle's gas tightness is high, and reinforced precision is high, and emulsification is efficient, and emulsification is effectual, and the product property of preparation can be good, and has realized the secondary recycle of solvent.

Description

Waterborne polyurethane dispersion apparatus for producing
Technical Field
The utility model relates to an aqueous polyurethane production technical field, concretely relates to aqueous polyurethane dispersion apparatus for producing.
Background
The synthesis reaction of the aqueous polyurethane resin involves the reaction of polyester polyol or polyether polyol with polyisocyanate, and since the polyether polyol contains a certain amount of moisture and the polyisocyanate can participate in the reaction with water to affect the reaction effect, the polyol needs to be subjected to vacuum dehydration treatment before the reaction. In the process of synthesizing the aqueous polyurethane resin, the polymer molecular weight gradually increases along with the progress of polymerization reaction, the molecular chain becomes longer, and the degree of molecular branching becomes larger, so that the viscosity of a polymer reaction system becomes larger and larger. In addition, in order to meet the environmental protection standard of the aqueous polyurethane dispersion, the solvent needs to be removed, and the volatile organic compounds of the product are reduced.
The existing production device generally adopts open feeding, air can be brought into a reaction system in the feeding process, and water contained in the air can influence the product quality when participating in the reaction. In addition, raw materials are easy to remain in a charging hopper or a pipeline during feeding, and the feeding precision is low. Therefore, in order to improve the product quality, the raw material feeding precision and the tightness of the reaction kettle need to be improved.
SUMMERY OF THE UTILITY MODEL
The to-be-solved technical problem of the utility model is: the production device for the aqueous polyurethane dispersion is high in air tightness of a polymerization reaction kettle, high in feeding accuracy, high in emulsification efficiency, good in emulsification effect, good in performance of prepared products, and capable of achieving secondary recycling of a solvent.
The device for producing the waterborne polyurethane dispersion comprises a polymerization reaction kettle, a high-speed dispersion kettle and a desolventizing kettle which are sequentially connected, wherein a feed inlet of the polymerization reaction kettle is connected with a monomer metering tank and an auxiliary agent metering tank, and discharge outlets of the monomer metering tank and the auxiliary agent metering tank are connected with a nitrogen purging pipeline; the top of the polymerization reaction kettle is provided with a condenser and an exhaust pipeline, and a discharge port is connected with a feed port of the high-speed dispersion kettle; two groups of dispersion discs and a group of stirrers are arranged in the high-speed dispersion kettle; the discharge hole of the high-speed dispersion kettle is connected with the feed inlet of the desolventizing kettle; the bottom of the desolventizing kettle is connected with a product output pipeline, and a top gas phase outlet is connected with a solvent recovery tank after passing through a cooler.
Preferably, the monomer metering tank is connected to the polyol line and the isocyanate line. In production, one or more polyether polyols are added into a monomer metering tank after being metered through a polyol pipeline, then the one or more polyether polyols are added into a polymerization reaction kettle, vacuum dehydration is carried out for 1 hour at 90 ℃, one or more isocyanates are added into the monomer metering tank through an isocyanate pipeline, after the temperature of the polyol in the polymerization reaction kettle is reduced to 80 ℃, the isocyanate in the monomer metering tank is added into the polymerization reaction kettle at a set flow rate, and materials are uniformly stirred under the action of a stirring device, so that the materials are uniformly heated, and polymerization reaction is carried out.
As a preferred scheme, the auxiliary agent metering tank is connected with a solvent pipeline and is provided with an auxiliary agent feeding port. In the polymerization reaction, a catalyst is required to be added in the early stage of the reaction to promote the reaction, a solvent is added in the middle stage of the reaction to adjust the viscosity of a polymerization reaction system, and a neutralizer is added in the later stage of the reaction to neutralize the reaction system. The catalyst and the neutralizing agent are added into an auxiliary agent metering tank through an auxiliary agent feeding port after being metered, then are added into a polymerization reaction kettle, and a proper amount of solvent is added into the auxiliary agent metering tank through a solvent pipeline after being added, and then are added into the polymerization reaction kettle, so that the catalyst or the neutralizing agent is prevented from remaining in the auxiliary agent metering tank and a pipeline; when the solvent is required to be added, the solvent is directly added into the auxiliary agent metering tank through the solvent pipeline and then added into the polymerization reaction kettle.
Wherein, the polyol pipeline, the isocyanate pipeline and the solvent pipeline are all provided with flow meters.
By arranging the monomer metering tank and the auxiliary agent metering tank, the relatively closed addition of reaction raw materials can be ensured, the air tightness of the polymerization reaction kettle is ensured, and the situation that the water in the air is mixed into a reaction system to participate in the reaction to influence the product quality because the feed inlet of the polymerization reaction kettle needs to be repeatedly opened when the raw materials are added is avoided; meanwhile, after the catalyst and the neutralizing agent are added into the auxiliary agent metering tank, the catalyst or the neutralizing agent is washed by the solvent, so that the residue of the catalyst or the neutralizing agent can be avoided, and the feeding accuracy is ensured.
The discharge ports of the monomer metering tank and the auxiliary agent metering tank are also connected with a nitrogen purging pipeline, and before feeding, nitrogen replacement and deoxidization can be carried out on the reaction device through the nitrogen purging pipeline; after feeding, can sweep the discharge pipeline of monomer metering tank and auxiliary agent metering tank through nitrogen gas sweep pipeline, make in the pipeline remaining raw materials all add polymerization cauldron, improve the accuracy nature of throwing the material.
As a preferable scheme, the polymerization reaction kettle, the high-speed dispersion kettle and the desolventizing kettle are reaction kettles with heating jackets and are provided with temperature sensors and pressure sensors, so that the temperature and the pressure in the kettles can be monitored in real time, and particularly, the system has a function of monitoring the pressure in real time in the vacuum dewatering and synthesis reaction stages. As a preferable scheme, the polymerization reaction kettle and the desolventizing kettle are provided with stirring devices, and any conventional stirring device can be selected.
As a preferable scheme, in the high-speed dispersing kettle, the stirring directions of the two groups of dispersing disks and the stirrer are opposite. Install two sets of dispersion impeller additional in the high-speed dispersion cauldron, increase emulsification in-process shearing force has better emulsification effect.
Wherein, the condenser arranged at the top of the polymerization reaction kettle plays a role in condensing and refluxing the solvent in the polymerization reaction, so that the viscosity of the polymer in the polymerization reaction is moderate and the reaction is uniform.
The desolventizing kettle can remove the volatile organic solvent in the aqueous polyurethane dispersion, so that the produced aqueous polyurethane dispersion meets the environmental protection requirement; the volatile organic solvent removed in the desolventizing kettle is cooled by a cooler and then enters a solvent recovery tank for secondary use.
The working process of the production device for the aqueous polyurethane dispersion is as follows:
before feeding in raw materials, nitrogen gas replacement deoxidization is carried out to reaction unit to nitrogen gas purge pipeline, after oxygen content is up to standard, add monomer metering tank after the polyol pipeline is measured with one or more polyether polyols earlier, add in the polymerization cauldron again, remove water 1 hour in vacuum under 90 ℃, add monomer metering tank with one or more isocyanate through the isocyanate pipeline simultaneously, after the polyol temperature drops to 80 ℃ in the polymerization cauldron, add the isocyanate in the monomer metering tank to the polymerization cauldron under setting for the flow, evenly stir the material under agitating unit's effect, make the material thermally equivalent, carry out polymerization. After reacting for 2 hours, the catalyst is added into an auxiliary agent metering tank through an auxiliary agent charging port after being metered, then is added into a polymerization reaction kettle, so that the polymerization reaction is more complete, and a proper amount of solvent is added into the auxiliary agent metering tank through a solvent pipeline after the catalyst is added, and then is added into the polymerization reaction kettle, so that the catalyst residue is avoided. And (3) continuing to react for 2 hours, adding the metered solvent into an auxiliary agent metering tank through a solvent pipeline, adding the solvent into a polymerization reaction kettle, adjusting the viscosity of the polymer to enable the reaction to be more uniform, and then, keeping the temperature at 80 ℃ for 1 hour. And cooling to 35 ℃, adding the measured neutralizer into the auxiliary agent measuring tank through the auxiliary agent feeding port, then adding the obtained product into the polymerization reaction kettle, adding a proper amount of solvent into the auxiliary agent measuring tank through the solvent pipeline after adding the neutralizer, and adding the obtained product into the polymerization reaction kettle to avoid the residue of the neutralizer. After the mixture is uniformly stirred, the waterborne polyurethane resin is introduced into a high-speed dispersion kettle, and is stirred under the combined action of a dispersion disc and a stirrer, so that the shearing force in the emulsification process is increased, and the emulsification effect is improved. Then, the aqueous polyurethane dispersion is led into a desolventizing kettle, the organic solvent is removed by reduced pressure distillation at 50 ℃, then the temperature of the product is reduced by 35 ℃ and the product is packaged through a product output pipeline, and the removed organic solvent enters a solvent recovery tank after being cooled by a cooler so as to be used for the second time.
Compared with the prior art, the utility model discloses following beneficial effect has:
(1) the utility model ensures the relatively airtight addition of reaction raw materials by arranging the monomer metering tank and the auxiliary agent metering tank, ensures the air tightness of the polymerization reaction kettle, avoids the need of repeatedly opening the charging hole of the polymerization reaction kettle when adding raw materials, and leads the moisture in the air to be mixed into the reaction system to participate in the reaction, thereby influencing the product quality; meanwhile, after the catalyst and the neutralizing agent are added into the auxiliary agent metering tank, the catalyst or the neutralizing agent is washed by the solvent, so that the residue of the catalyst or the neutralizing agent can be avoided, and the feeding accuracy is ensured;
(2) the utility model arranges the nitrogen purging pipeline at the discharge outlets of the monomer metering tank and the auxiliary agent metering tank, and can perform nitrogen replacement deoxidization on the reaction device through the nitrogen purging pipeline before feeding; after feeding, the discharge pipelines of the monomer metering tank and the auxiliary agent metering tank can be swept through the nitrogen sweeping pipeline, so that the raw materials remained in the pipelines are all added into the polymerization reaction kettle, and the feeding accuracy is improved;
(3) the utility model adds two groups of dispersion discs in the high-speed dispersion kettle, increases the shearing force in the emulsification process, greatly improves the emulsification efficiency and has good emulsification effect;
(4) the utility model discloses an aqueous polyurethane dispersion apparatus for producing, easy operation, production efficiency is high, and the product of preparation can be good, and has realized the secondary recycle of solvent.
Drawings
FIG. 1 is a schematic structural view of an apparatus for producing an aqueous polyurethane dispersion according to the present invention;
in the figure: 1. a polyol line; 2. an isocyanate line; 3. a solvent line; 4. a monomer metering tank; 5. an additive charging port; 6. an additive metering tank; 7. purging the pipeline with nitrogen; 8. an exhaust line; 9. a condenser; 10. a polymerization reaction kettle; 11. a dispersion tray; 12. a stirrer; 13. a high-speed dispersion kettle; 14. a desolventizing kettle; 15. a product output pipeline; 16. a cooler; 17. and a solvent recovery tank.
Detailed Description
The following will describe in detail specific embodiments of the present invention. Well-known structures or functions may not be described in detail in the following embodiments in order to avoid unnecessarily obscuring the details. Approximating language, as used herein in the following examples, may be applied to identify quantitative representations that could permissibly vary in number without resulting in a change in the basic function. Unless defined otherwise, technical and scientific terms used in the following examples have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
Example 1
As shown in fig. 1, the apparatus for producing aqueous polyurethane dispersion of the present invention comprises a polymerization reactor 10, a high-speed dispersion reactor 13 and a desolventizing reactor 14, which are connected in sequence, wherein a feed inlet of the polymerization reactor 10 is connected with a monomer metering tank 4 and an auxiliary agent metering tank 6, and a discharge outlet of the monomer metering tank 4 and the auxiliary agent metering tank 6 is connected with a nitrogen purging pipeline 7; the top of the polymerization reaction kettle 10 is provided with a condenser 9 and an exhaust pipeline 8, and a discharge hole is connected with a feed inlet of a high-speed dispersion kettle 13; two groups of dispersion discs 11 and a group of stirrers 12 are arranged in the high-speed dispersion kettle 13; the discharge hole of the high-speed dispersion kettle 13 is connected with the feed hole of the desolventizing kettle 14; the bottom of the desolventizing kettle 14 is connected with a product output pipeline 15, and a top gas phase outlet passes through a cooler 16 and then is connected with a solvent recovery tank 17.
Preferably, the monomer metering tank 4 is connected to the polyol line 1 and the isocyanate line 2. In production, firstly, one or more polyether polyols are added into a monomer metering tank 4 after being metered through a polyol pipeline 1, then the polyether polyols are added into a polymerization reaction kettle 10, vacuum dehydration is carried out for 1 hour at 90 ℃, one or more isocyanates are added into the monomer metering tank 4 through an isocyanate pipeline 2, after the temperature of the polyol in the polymerization reaction kettle 10 is reduced to 80 ℃, the isocyanate in the monomer metering tank 4 is added into the polymerization reaction kettle 10 at a set flow rate, and materials are uniformly stirred under the action of a stirring device, so that the materials are uniformly heated, and polymerization reaction is carried out.
As a preferable scheme, the auxiliary agent metering tank 6 is connected with the solvent pipeline 3 and is provided with an auxiliary agent feeding port 5. In the polymerization reaction, a catalyst is required to be added in the early stage of the reaction to promote the reaction, a solvent is added in the middle stage of the reaction to adjust the viscosity of a polymerization reaction system, and a neutralizer is added in the later stage of the reaction to neutralize the reaction system. Wherein the catalyst and the neutralizing agent are added into an auxiliary agent metering tank 6 through an auxiliary agent feeding port 5 after being metered, then are added into a polymerization reaction kettle 10, and then are added into the auxiliary agent metering tank 6 through a solvent pipeline 3, and then are added into the polymerization reaction kettle 10, so that the catalyst or the neutralizing agent is prevented from remaining in the auxiliary agent metering tank 6 and a pipeline; when the solvent is required to be added, the solvent is directly added into the auxiliary agent metering tank 6 through the solvent pipeline 3 and then is added into the polymerization reaction kettle 10.
Wherein, the polyol pipeline 1, the isocyanate pipeline 2 and the solvent pipeline 3 are all provided with flow meters.
By arranging the monomer metering tank 4 and the auxiliary agent metering tank 6, the relatively airtight addition of reaction raw materials can be ensured, the air tightness of the polymerization reaction kettle 10 is ensured, and the situation that the water in the air is mixed into a reaction system to participate in the reaction to influence the product quality because the feed inlet of the polymerization reaction kettle 10 needs to be repeatedly opened when the raw materials are added is avoided; meanwhile, after the catalyst and the neutralizing agent are added into the auxiliary agent metering tank 6, the catalyst or the neutralizing agent is washed by the solvent, so that the residue of the catalyst or the neutralizing agent can be avoided, and the feeding accuracy is ensured.
The discharge ports of the monomer metering tank 4 and the auxiliary agent metering tank 6 are also connected with a nitrogen purging pipeline 7, and before feeding, nitrogen displacement deoxygenation can be carried out on the reaction device through the nitrogen purging pipeline 7; after feeding, the discharge pipelines of the monomer metering tank 4 and the auxiliary agent metering tank 6 can be swept through the nitrogen sweeping pipeline 7, so that residual raw materials in the pipelines are added into the polymerization reaction kettle 10, and the feeding accuracy is improved.
As a preferable scheme, the polymerization reaction kettle 10, the high-speed dispersing kettle 13 and the desolventizing kettle 14 are reaction kettles with heating jackets and are provided with temperature sensors and pressure sensors, so that the temperature and the pressure in the kettles can be monitored in real time, and particularly, the real-time pressure monitoring function is realized in the vacuum dewatering and synthesis reaction stages. As a preferable mode, the polymerization reactor 10 and the desolventizing reactor 14 are provided with stirring devices, and any conventional stirring device can be selected.
In the high-speed dispersing tank 13, the two dispersing disks 11 and the stirrer 12 are preferably stirred in opposite directions. Install two sets of dispersion impeller 11 additional in high-speed dispersion tank 13, increase emulsification in-process shearing force, have better emulsification effect.
Wherein, the condenser 9 arranged at the top of the polymerization reaction kettle 10 plays a role of condensing and refluxing the solvent in the polymerization reaction, so that the polymer has moderate viscosity and uniform reaction in the polymerization reaction.
The desolventizing kettle 14 can remove the volatile organic solvent in the aqueous polyurethane dispersion, so that the produced aqueous polyurethane dispersion meets the environmental protection requirement; the volatile organic solvent removed in the desolventizing kettle 14 is cooled by a cooler 16 and then enters a solvent recovery tank 17 for secondary use.
The working process of the production device for the aqueous polyurethane dispersion is as follows:
before feeding, nitrogen gas replacement deoxidization is carried out to reaction unit to nitrogen gas purge line 7, after oxygen content is up to standard, add monomer metering tank 4 with one or more polyether polyol through polyol pipeline 1 after the measurement earlier, add in polymerization cauldron 10 again, vacuum dehydration 1 hour at 90 ℃, add monomer metering tank 4 with one or more isocyanate through isocyanate pipeline 2 simultaneously, after the polyol temperature in polymerization cauldron 10 reduces to 80 ℃, add the isocyanate in monomer metering tank 4 to polymerization cauldron 10 under the settlement flow, evenly stir the material under agitating unit's effect, make the material thermally equivalent, carry out polymerization. After reacting for 2 hours, the catalyst is added into an auxiliary agent metering tank 6 through an auxiliary agent charging port 5 after being metered, then is added into a polymerization reaction kettle 10, so that the polymerization reaction is more complete, and a proper amount of solvent is added into the auxiliary agent metering tank 6 through a solvent pipeline 3 after the catalyst is added, and then is added into the polymerization reaction kettle 10, so that the catalyst residue is avoided. And (3) continuing to react for 2 hours, adding the metered solvent into an auxiliary agent metering tank 6 through a solvent pipeline 3, then adding the solvent into a polymerization reaction kettle 10 for adjusting the viscosity of the polymer to enable the reaction to be more uniform, and then, preserving the heat at 80 ℃ for 1 hour. Cooling to 35 ℃, adding the measured neutralizer into an auxiliary agent measuring tank 6 through an auxiliary agent feeding port 5, then adding the obtained product into a polymerization reactor 10, adding a proper amount of solvent into the auxiliary agent measuring tank 6 through a solvent pipeline 3 after adding the neutralizer, and then adding the obtained product into the polymerization reactor 10 to avoid the residual neutralizer. After the mixture is uniformly stirred, the waterborne polyurethane resin is introduced into a high-speed dispersion kettle 13, and is stirred under the combined action of a dispersion plate 11 and a stirrer 12, so that the shearing force in the emulsification process is increased, and the emulsification effect is improved. Then, the aqueous polyurethane dispersion is led into a desolventizing kettle 14, organic solvent is removed by reduced pressure distillation at 50 ℃, then the temperature of the product is reduced by 35 ℃, the product is packaged through a product output pipeline 15, and the removed organic solvent enters a solvent recovery tank 17 after being cooled by a cooler 16 so as to be used for the second time.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments described in the foregoing embodiments, or equivalents may be substituted for elements thereof. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (6)

1. An aqueous polyurethane dispersion production device is characterized in that: the device comprises a polymerization reaction kettle (10), a high-speed dispersion kettle (13) and a desolventizing kettle (14) which are sequentially connected, wherein a feed inlet of the polymerization reaction kettle (10) is connected with a monomer metering tank (4) and an auxiliary agent metering tank (6), and discharge outlets of the monomer metering tank (4) and the auxiliary agent metering tank (6) are connected with a nitrogen purging pipeline (7); a condenser (9) and an exhaust pipeline (8) are arranged at the top of the polymerization reaction kettle (10), and a discharge hole is connected with a feed inlet of a high-speed dispersion kettle (13); a dispersion disc (11) and a stirrer (12) are arranged in the high-speed dispersion kettle (13); the discharge hole of the high-speed dispersion kettle (13) is connected with the feed hole of the desolventizing kettle (14); the bottom of the desolventizing kettle (14) is connected with a product output pipeline (15), and a top gas phase outlet is connected with a solvent recovery tank (17) after passing through a cooler (16).
2. The apparatus for producing an aqueous polyurethane dispersion according to claim 1, wherein: the monomer metering tank (4) is connected with the polyol pipeline (1) and the isocyanate pipeline (2).
3. The apparatus for producing an aqueous polyurethane dispersion according to claim 1, wherein: the auxiliary agent metering tank (6) is connected with the solvent pipeline (3) and is provided with an auxiliary agent feeding port (5).
4. The apparatus for producing an aqueous polyurethane dispersion according to claim 1, characterized in that: the polymerization reaction kettle (10), the high-speed dispersion kettle (13) and the desolventizing kettle (14) are reaction kettles with heating jackets and are provided with temperature sensors and pressure sensors.
5. The apparatus for producing an aqueous polyurethane dispersion according to claim 1, characterized in that: two groups of dispersion discs (11) and a group of stirrers (12) are arranged in the high-speed dispersion kettle (13).
6. The apparatus for producing an aqueous polyurethane dispersion according to claim 1 or 5, characterized in that: in the high-speed dispersion kettle (13), the stirring directions of the two groups of dispersion discs (11) and the stirrer (12) are opposite.
CN202220527199.3U 2022-03-11 2022-03-11 Waterborne polyurethane dispersion apparatus for producing Active CN217313359U (en)

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CN202220527199.3U CN217313359U (en) 2022-03-11 2022-03-11 Waterborne polyurethane dispersion apparatus for producing

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Application Number Priority Date Filing Date Title
CN202220527199.3U CN217313359U (en) 2022-03-11 2022-03-11 Waterborne polyurethane dispersion apparatus for producing

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