Preparation device and method of polyurea viscosifier powder

Through the continuous spray reaction and solvent separation and recovery device, the problems of difficult stirring and incomplete solvent evaporation in the preparation process of polyurea thickener powder are solved, and efficient continuous production and preparation of high-performance grease are achieved.

CN116617998BActive Publication Date: 2025-10-17CHINA PETROLEUM & CHEMICAL CORP +1
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Patent Information

Application Number
CN202310634872.2
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-05-31
Publication Date
2025-10-17
Estimated Expiration
2043-05-31

AI Technical Summary

Technical Problem

In the prior art, the preparation process of polyurea thickener powder has problems such as difficult stirring, incomplete solvent evaporation and soap powder agglomeration, which affect the use effect.

Method used

A continuous spray reaction, solvent separation and recovery device is used to prepare polyurea thickener powder through spray contact, and the solvent is quickly separated and recovered under hot air and cyclone separation devices to solve the problems of difficult stirring and incomplete solvent evaporation.

Benefits of technology

The efficient and continuous production of polyurea thickener powder was achieved, solving the problems of difficult stirring, incomplete solvent evaporation and soap powder agglomeration. The performance of the prepared grease was comparable to that of the traditional method.

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Abstract

The application relates to the technical field of polyurea grease preparation devices and processes, in particular to a polyurea thickener powder preparation device and method, which comprises a spraying reaction system, a solvent separation system and a solvent recovery system; the solvent separation system comprises a hot air conveying device and a cyclone separation device; the solvent recovery system is arranged at the top of the cyclone separation device; the hot air conveying device blows the polyurea thickener prepared by the spraying reaction system into the cyclone separation device, and the solvent is evaporated and then enters the solvent recovery system. The polyurea thickener powder preparation device and method provided by the application solve the problems of stirring difficulty, incomplete solvent evaporation, soap powder caking and use influence in the preparation process of the prefabricated polyurea thickener powder, and the prepared polyurea thickener powder can obtain lubricating grease with performance equivalent to that prepared by a traditional method.
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Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of polyurea grease preparation process and device, and particularly relates to a polyurea thickener powder preparation device and method. BACKGROUND

[0002] With the rapid development of modern industry, for the mechanical equipment running at high speed under high load and high temperature, the high temperature use range of the lubricating grease reaches 175-235 DEG C or even higher, and a higher service life is required. The polyurea grease is a kind of lubricating grease with organic polymer as thickener, which is different from the metal soap-based thickener, avoids the catalytic oxidation of metal ions to the base oil of the lubricating grease, has good oxidation stability, thermal stability, pumping property, mechanical stability and colloidal stability, and is particularly suitable for high temperature, high load and wide temperature range occasions, and is a kind of multi-purpose high performance lubricating grease.

[0003] At present, the polyurea grease is produced by the "in situ" method, that is, the amine reacts with isocyanate in the base oil to generate the polyurea thickener, and the base oil is thickened to obtain the polyurea grease. However, the isocyanate has strict requirements on the storage temperature, and is prone to deterioration due to the generation of dimer at room temperature for a long time. The treatment of isocyanate brings considerable technical problems to the lubricating grease manufacturers. In addition, because the polyaddition reaction is an exothermic reaction, the internal temperature of the reaction material may also be non-uniform, and problems may also occur when removing heat. Although the metal soap-based lubricating grease has technical advantages, this fact has a negative impact on the further promotion of the polyurea grease.

[0004] The pre-prepared polyurea thickener powder provides a non-toxic and harmless, convenient transportation and storage, environmentally friendly and safe intermediate raw material for the production of polyurea grease, reduces the threshold and cost of polyurea grease production, and provides a material basis for stabilizing and improving the quality of polyurea grease and upgrading lubricating grease products.

[0005] In order to overcome the technical problem of the difficulty in storing isocyanate, patent EP0534248A1 develops a method for obtaining polyurea thickener by extrusion in a solvent or non-solvent, drying and grinding to obtain pre-prepared polyurea thickener powder. Then the pre-prepared thickener powder is mixed with the base oil, and the polyurea grease is obtained by rolling oil treatment. Patents CN100378209C, CN101440329A, CN110437912A, CN1465680A and CN110499202A respectively disclose a method for stirring the raw materials dissolved in ethanol, inert solvent, chlorobenzene, water and ethyl acetate, and obtaining dry pre-prepared polyurea soap powder by vacuumizing and heating the reactor after reaction.

[0006] A method for preparing preformed polyurea thickener by spray drying was disclosed by Evonik Resource Efficiency GmbH (patent DE102004044878.7): the mixed stirring obtained polyurea powder suspension was spray dried under the protection of nitrogen as protective gas, under suitable atomization pressure and temperature to obtain dry polyurea thickener powder.

[0007] However, the above prior art still has the problems of difficult stirring caused by solvent evaporation during the preparation of polyurea thickener powder, safety hazard of deflagration caused by solvent evaporation, and blockage of soap powder affecting use caused by incomplete solvent evaporation.

[0008] Therefore, it is necessary to provide an improved preparation device and method for polyurea thickener powder to solve the above problems. SUMMARY

[0009] The purpose of the present application is to provide a preparation device and method for polyurea thickener powder, which uses continuous spray reaction, solvent separation and recovery device, and prepares polyurea thickener powder by spray contact of amine and isocyanate in the presence of solvent, followed by rapid separation and recovery of solvent under hot air and cyclone separation device, effectively solving the problems of difficult stirring, incomplete solvent evaporation and blockage of soap powder.

[0010] To achieve the above purpose, the present application provides a preparation device for polyurea thickener powder, comprising a spray reaction system, a solvent separation system and a solvent recovery system.

[0011] The solvent separation system comprises a hot air conveying device and a cyclone separation device; the solvent recovery system is arranged at the top of the cyclone separation device.

[0012] The hot air conveying device blows the polyurea thickener prepared by the spray reaction system into the cyclone separation device, and the solvent evaporates into the solvent recovery system, and the polyurea thickener powder is separated.

[0013] Further, the solvent separation system further comprises a sealed cavity connected to the spray reaction system and the cyclone separation device respectively, and the hot air conveying device is arranged in the sealed cavity.

[0014] And / or, the hot air conveying device is arranged below the spray reaction system, and the conveying direction of hot air is perpendicular to the discharging direction of the spray reaction system.

[0015] Further, the hot air conveying device comprises a blower and a heating device.

[0016] And / or, the solvent separation system further comprises a collection tank arranged below the cyclone separation device, for collecting the polyurea thickener powder.

[0017] Furthermore, the spray reaction system includes a spray reaction tank connected to the solvent separation system, an amine liquid spray device, and an isocyanate spray device; the amine liquid spray device and the isocyanate spray device are both arranged inside the spray reaction tank.

[0018] Furthermore, the amine liquid spray device and the isocyanate spray device are respectively arranged on two opposite side walls of the spray reaction tank, and include a plurality of spray guns arranged along the height direction of the side walls.

[0019] Furthermore, the spray reaction system further comprises an amine dissolving tank and an isocyanate dissolving tank; an amine liquid booster pump is provided between the amine dissolving tank and the amine liquid spraying device; an isocyanate booster pump is provided between the isocyanate dissolving tank and the isocyanate spraying device;

[0020] The pressure adjustment range of the amine liquid booster pump and the isocyanate booster pump is 0-1 MPa.

[0021] Furthermore, the solvent recovery system includes a solvent collecting device and a condensing device;

[0022] The solvent collection device includes a solvent flow area, a solvent recovery area and a solvent condensation area; the solvent flow area is sealed and connected to the top of the cyclone separation device; the solvent recovery area is vertically connected to the solvent flow area; the solvent condensation area is vertically connected to the solvent recovery area, and a solvent outlet is provided at the bottom of the solvent condensation area; the condensation device is arranged in the solvent condensation area.

[0023] Furthermore, a temperature sensor is provided on the top of the solvent collecting device;

[0024] And / or, the condensing medium of the condensing device includes cooling water or chilled brine; the flow direction of the condensing medium is opposite to the outflow direction of the solvent.

[0025] In a second aspect, the present invention further provides a method for preparing polyurea thickener powder, using any of the preparation devices described above, comprising:

[0026] S1, preheating the reaction zone of the spray reaction system and the separation zone of the solvent separation system;

[0027] S2. Amine and isocyanate are simultaneously sprayed into the reaction zone to carry out a contact reaction; the reaction product downwardly enters the solvent separation system and, under the action of the hot air conveying device, enters the cyclone separation device; after separation, the solvent enters the solvent recovery system to achieve separation and recovery; the reaction product enters the lower discharge port of the cyclone separation device.

[0028] Furthermore, in step S1, the preheating temperature of the reaction zone is 50-70°C, and the preheating temperature of the separation zone is 110-130°C;

[0029] And / or, in step S2, the amine is one or more of aliphatic amines and aromatic amines, preferably one or more of octylamine, dodecylamine, hexadecylamine, octadecylamine, aniline, p-toluidine, cyclohexylamine, dicyclohexylamine, p-chloroaniline, m-phenylenediamine, p-phenylenediamine, o-phenylenediamine, melamine, dibenzimidazole diamine, and benzidine;

[0030] The isocyanate is one of monoisocyanate, diisocyanate or polyisocyanate, preferably one or more of toluene diisocyanate, isophorone diisocyanate, diphenylmethane diisocyanate, dicyclohexylmethane diisocyanate, hexamethylene diisocyanate and lysine diisocyanate;

[0031] The solvent is a low-boiling base oil or an organic solvent, preferably one or more of ethyl acetate, toluene, acetone, chloroform, benzene, and petroleum ether;

[0032] The total weight of the amine and the isocyanate is 10% to 85% of the total weight of the solvent.

[0033] The beneficial effects of the present invention are as follows:

[0034] The polyurea thickener powder preparation device provided by the present invention is a continuous and efficient polyurea production device that solves the problems encountered during the preparation of prefabricated polyurea thickener powder, such as difficult stirring, incomplete solvent evaporation, and soap powder agglomeration, which hinder its usability. This device enables industrial, continuous production of prefabricated polyurea thickener powder, not only enhancing its technological impact in the field but also achieving high economic benefits.

[0035] 2. The present invention provides a method for preparing a polyurea thickener powder. Amines and isocyanates are contacted by spraying in the presence of a solvent to prepare the polyurea thickener. The polyurea thickener is then dried and separated under hot air flow, and then collected in a solvent recovery system to form a preformed polyurea thickener powder. Grease produced using this preformed polyurea thickener powder exhibits comparable performance to grease produced by conventional methods. BRIEF DESCRIPTION OF THE DRAWINGS

[0036] In order to more clearly illustrate the technical solutions in the present invention or the prior art, the following briefly introduces the drawings required for use in the embodiments or the description of the prior art. Obviously, the drawings described below are some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative work.

[0037] Figure 1is a structural schematic diagram of a preparation device of polyurea thickening agent powder provided by the present application;

[0038] Figure 2 is a physical map of polyurea thickening agent powder prepared by the present application and comparative examples;

[0039] Reference signs:

[0040] 10-spray reaction system; 11-spray reaction tank; 12-amine dissolving tank; 13-isocyanate dissolving tank; 14-amine liquid booster pump; 15-isocyanate booster pump; 16-amine liquid spraying device; 17-isocyanate spraying device; 20-solvent separation system; 21-blower; 22-heating device; 23-cyclone separation device; 24-collection tank; 25-sealing cavity; 30-solvent recovery system; 31-solvent collection device; 32-condensing device; 33-solvent outlet; 34-temperature sensor. DETAILED DESCRIPTION

[0041] In order to make the objects, technical solutions and advantages of the present application clearer, the technical solutions in the present application are described clearly and completely below. Obviously, the described embodiments are some of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor fall within the protection scope of the present application.

[0042] Please refer to Figure 1 As shown in the figure, the present application provides a preparation device of polyurea thickening agent powder, which comprises a spray reaction system 10, a solvent separation system 20 and a solvent recovery system 30. The solvent separation system 20 comprises a hot air conveying device and a cyclone separation device 23; the solvent recovery system 20 is arranged at the top of the cyclone separation device 23. The hot air conveying device blows the polyurea thickening agent prepared by the spray reaction system 10 into the cyclone separation device 23, and the solvent evaporates and enters the solvent recovery system 30.

[0043] Specifically, the polyurea thickening agent is prepared by spraying the contact of amine and isocyanate in the presence of solvent, the polyurea thickening agent enters the cyclone separation device 23 through the hot air conveying device, the pre-prepared polyurea thickening agent powder is collected at the lower part of the cyclone separation device 23, the solvent is separated from the pre-prepared polyurea thickening agent powder and enters the solvent recovery area from the upper part of the cyclone separation device 23, and is collected after condensation for recycling.

[0044] Thus, the point-to-point reaction through the spray contact can solve the stirring difficulty, and the contact reaction efficiency is high, and the reaction product is still in the form of dispersed particles. Since the raw materials of the polyurea thickening agent powder are mostly solids, the spray contact reaction is carried out after the raw materials are dissolved in the solvent. The hot air device below the spray reaction system 10 can transport the product to the cyclone separation device 23, and the heat can help the solvent to evaporate, and can prolong the contact reaction time of the raw materials to ensure the complete reaction. Under the centrifugal force of the cyclone separation device 23, the solvent and the product particles are effectively separated, and the dry product particles are not easy to be agglomerated, so the problems of stirring difficulty, incomplete solvent evaporation, soap powder agglomeration, and difficult solvent recovery are solved.

[0045] Specifically, the solvent separation system 20 further comprises a sealed cavity 25 connected with the spray reaction system 10 and the cyclone separation device 23 respectively, and the hot air conveying device is arranged in the sealed cavity 25. Thus, the spray reaction system 10 and the cyclone separation device 23 are arranged in a sealed and continuous manner, which can help to realize continuous production, and can prevent the materials from being oxidized or contaminated. The devices can be connected through flanges. The reaction product is settled downward into the sealed cavity 25, and then is conveyed to the cyclone separation device 23, which can prolong the contact reaction time of the materials to ensure the complete reaction of the raw materials. Moreover, during the hot air blowing stage, the product particles that have not been completely reacted are in a mixed state of solid product and liquid raw material, and the liquid raw material can still be fully contacted and reacted. Therefore, the device is a high-efficiency and high-yield continuous preparation device for polyurea thickening agent powder.

[0046] In particular, the hot air conveying device is arranged on the lower side of the spray reaction system, and the conveying direction of the hot air is perpendicular to the discharging direction of the spray reaction system. Thus, the reaction product is settled downward under the action of gravity, and the hot air from the side blows it forward to the entrance of the cyclone separation device 23. The blowing distance of the product can be adjusted by adjusting the distance between the hot air conveying device and the cyclone separation device 23, so as to ensure sufficient time for complete reaction.

[0047] In some specific embodiments, the hot air conveying device comprises a blower 21 and a heating device 22, and the heating device 22 is arranged at the outlet of the blower 21 to heat the air blown by the blower 21. By adjusting the temperature and the amount of the hot air, the evaporation intensity of the solvent and the discharging speed of the product can be adjusted.

[0048] The solvent separation system 20 further comprises a collection tank 24 arranged below the cyclone separation device 23, for collecting the polyurea thickening agent powder.

[0049] The solvent separation system 20 solves the problems of incomplete solvent evaporation and soap powder agglomeration in the preparation process of the prefabricated polyurea thickening agent powder.

[0050] Specifically, the spray reaction system 10 comprises a spray reaction tank 11 connected with the solvent separation system 20, and an amine liquid spray device 16 and an isocyanate spray device 17; the amine liquid spray device 16 and the isocyanate spray device 17 are both arranged in the interior of the spray reaction tank 11. In particular, the amine liquid spray device 16 and the isocyanate spray device 17 are arranged on two opposite side walls of the spray reaction tank 11, respectively, and each comprises a plurality of spray guns arranged along the height direction of the side wall. In this way, the amine liquid and the isocyanate atomized droplets are sprayed into the spray reaction tank 11 oppositely, and then collide and contact to react, so that the contact efficiency is higher.

[0051] The spray reaction system 10 further comprises an amine dissolving tank 12 and an isocyanate dissolving tank 13; an amine liquid booster pump 14 is arranged between the amine dissolving tank 12 and the amine liquid spray device 16; an isocyanate booster pump 15 is arranged between the isocyanate dissolving tank 13 and the isocyanate spray device 17; the pressure adjustment range of the amine liquid booster pump 14 and the isocyanate booster pump 15 is 0-1 MPa. By adjusting the pressure to change the contact efficiency of the amine liquid and the isocyanate in the reaction zone, the problem of difficult stirring in the preparation process of the pre-made polyurea thickening agent powder is solved.

[0052] Specifically, the solvent recovery system 30 comprises a solvent collecting device 31 and a condensing device 32; and is used for condensing and recycling the solvent.

[0053] The solvent collecting device 31 comprises a solvent flow area, a solvent recovery area and a solvent condensing area; the solvent flow area is sealingly connected with the top of the cyclone separation device; the solvent recovery area is vertically connected with the solvent flow area; the solvent condensing area is vertically connected with the solvent recovery area, and the bottom of the solvent condensing area is provided with a solvent outlet 33; and the condensing device 32 is arranged in the solvent condensing area. In this way, the condensation and recovery of the solvent are facilitated, and the condensed solvent can be prevented from flowing back to the cyclone separation device 23.

[0054] In particular, the top of the solvent collecting device 31 is provided with a temperature sensor 34; and is used for detecting the temperature of the solvent evaporated into the solvent recovery system 30.

[0055] The condensing medium of the condensing device 32 comprises cooling water or refrigerated brine; and the flow direction of the condensing medium is opposite to the outflow direction of the solvent. The condensing device 32 selects the condensing medium according to the selected solvent, so that the problem of difficult solvent recovery in the solvent recovery process of the pre-made polyurea thickening agent powder is solved.

[0056] In a second aspect, the present application further provides a preparation method of a polyurea thickening agent powder, which adopts the preparation device of any one of the above aspects, and comprises the following steps:

[0057] S1, preheating the reaction zone of the spray reaction system and the separation zone of the solvent separation system;

[0058] S2, synchronously spraying the amine and the isocyanate into the reaction zone to perform a contact reaction; the reaction product enters the solvent separation system downward and enters the cyclone separation device under the action of the hot air conveying device; after the reaction solvent is separated, it enters the solvent recovery system to realize separation and recovery; the reaction product enters the lower discharge port of the cyclone separation device.

[0059] Specifically, in step S1, the preheating temperature of the reaction zone is 50-70℃, and the preheating temperature of the separation zone is 110-130℃; the temperature of the reaction zone should not be too high, otherwise the solvent will evaporate too fast, which will affect the yield of the contact reaction. The temperature of the separation zone is moderate, which can promote the volatilization of the solvent on the one hand and prevent the destruction of the structure of the pre-prepared polyurea thickener powder on the other hand.

[0060] In step S2, the amine is one or more of aliphatic amine and aromatic amine, preferably one or more of octylamine, dodecylamine, hexadecylamine, octadecylamine, aniline, p-toluidine, cyclohexylamine, dicyclohexylamine, p-chloroaniline, m-phenylenediamine, p-phenylenediamine, o-phenylenediamine, melamine, diphenyl imidazole diamine, and benzidine;

[0061] The isocyanate is one of monoisocyanate, diisocyanate or polyisocyanate, preferably one or more of toluene diisocyanate, isophorone diisocyanate, diphenyl methane diisocyanate, dicyclohexyl methane diisocyanate, hexamethylene diisocyanate, and lysine diisocyanate;

[0062] The solvent is one or more of low-boiling base oil or organic solvent, preferably one or more of ethyl acetate, toluene, acetone, chloroform, benzene, and petroleum ether.

[0063] The total weight of the amine and the isocyanate is 10%-85% of the total weight of the solvent. The concentration should not be too large, otherwise the raw materials in each atomized droplet will be too much, which may lead to incomplete contact reaction and large product particles, affecting the purity and dispersibility of the product. If the concentration is too small, the amount of solvent used will increase, which will increase the cost and affect the production efficiency. The present application can control the concentration of raw materials to regulate the reaction efficiency, yield and product particle size, so as to prepare the target optimized product.

[0064] Example 1

[0065] Ethyl acetate 90 kg was added to the amine tank in advance, stirring was started and the temperature was raised to 70℃, then 11.3 kg of octadecylamine was added, and after the octadecylamine was completely dissolved, 23.6 kg of cyclohexylamine was added. Ethyl acetate 90 kg was added to the MDI tank in advance, stirring was started and the temperature was raised to 70℃, then 30.03 kg of diphenyl methane diisocyanate was added.

[0066] Meanwhile, the reaction zone of the spray reaction tank 11 and the separation zone of the solvent separation system 20 are preheated to 60℃ and 120℃ respectively. The amine liquid booster pump and the MDI liquid booster pump are turned on to make the amine liquid and the MDI liquid contact and react in the form of spray in the reaction zone. The reaction product is separated in the cyclone separation device after being heated in the separation zone. The solvent ethyl acetate is collected from the upper part of the cyclone separation device 23 and recycled after being collected by the solvent recovery system 30. The dry preformed polyurea thickening agent powder is collected from the lower part of the cyclone separation device 23 and filled. The sample is tested by infrared, and no 2270cm -1 MDI characteristic absorption peak, which shows that the preparation device of the polyurea thickening agent powder provided by the application, the continuous arrangement of the spray reaction system, the solvent separation system and the solvent recovery system is reasonable, which can ensure complete spray contact and reaction and obtain high-purity product.

[0067] Comparative Example 1

[0068] A beaker is weighed with 180g of ethyl acetate, 22.6g of octadecylamine is dissolved at 71℃, and 47.2g of cyclohexylamine is added after cooling to 67℃; the reaction kettle is pre-filled with 180g of ethyl acetate and 70.1g of diphenylmethane diisocyanate, and the conductive oil is heated to 60℃; after both are completely dissolved, the amine liquid is added to the kettle. The amine liquid is introduced, and the reaction kettle reacts instantaneously. The temperature in the reaction kettle rises to 92℃, a large amount of gas evaporates, and the kettle presents a wet powder state, making stirring difficult. The sample is tested by infrared, and no 2270cm -1 MDI characteristic absorption peak. The conductive oil is heated to 140℃ and kept for 2 hours to evaporate most of the solvent ethyl acetate, and the preformed polyurea thickening agent powder is collected.

[0069] The photos of the preformed polyurea thickening agent powders obtained in the examples and comparative examples are shown in Figure 2 The preformed polyurea thickening agent powders obtained in the examples and comparative examples are respectively added to base oil and heated to 120℃ to prepare a 12wt% concentration suspension. After being ground and homogenized by a three-roll mill, the corresponding lubricating grease is obtained. The performance comparison of the lubricating grease products is shown in Table 1.

[0070] The above examples and comparative examples show that the preformed polyurea thickening agent powder preparation device and method provided by the application solve the problems of difficult stirring, incomplete solvent evaporation, soap powder caking and the like in the preparation process of the preformed polyurea thickening agent powder, and the performance of the lubricating grease prepared from the preformed polyurea thickening agent powder is equivalent to that of the lubricating grease produced by the traditional method.

[0071] Table 1 Lubricating grease performance comparison

[0072] Indicator Example Comparative Example Taper, 0.1 mm 285 297 Working taper, 0.1 mm 297 305 Extended working taper, 0.1 mm 352 378 Drop point, °C 292 295

[0073] It should be pointed out finally that the above embodiments are only used to illustrate the technical solutions of the present application, but not to limit the same; and although the present application has been described in detail with reference to the foregoing embodiments, it should be appreciated by those skilled in the art that the technical solutions recorded in the foregoing embodiments can be modified, or some technical features thereof can be replaced equivalently; and these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the spirit and scope of the technical solutions of the embodiments of the present application.

Claims

1. A method for preparing polyurea thickener powder, characterized in that: The device used in the preparation method includes a spray reaction system, a solvent separation system and a solvent recovery system; The solvent separation system includes a hot air conveying device and a cyclone separation device; the solvent recovery system is arranged on the top of the cyclone separation device; The hot air conveying device blows the polyurea thickener produced by the spray reaction system into the cyclone separation device, and the solvent enters the solvent recovery system after evaporation to separate and obtain polyurea thickener powder; The spray reaction system includes a spray reaction tank connected to the solvent separation system, an amine liquid spray device, and an isocyanate spray device; the amine liquid spray device and the isocyanate spray device are both arranged inside the spray reaction tank; The amine liquid spray device and the isocyanate spray device are respectively arranged on two opposite side walls of the spray reaction tank, and include a plurality of spray guns arranged along the height direction of the side walls, so that the atomized droplets of the amine liquid and the isocyanate are sprayed into the spray reaction tank oppositely, and then a collision contact reaction occurs; The solvent separation system further comprises a sealed cavity connected to the spray reaction system and the cyclone separation device respectively, and the hot air conveying device is arranged in the sealed cavity; And / or, the hot air conveying device is arranged below the spray reaction system; The spray reaction system further comprises an amine dissolving tank and an isocyanate dissolving tank, both of which are filled with solvent; S1, preheating the reaction zone of the spray reaction system and the separation zone of the solvent separation system; S2. Synchronously spraying an amine solution and an isocyanate solution into the reaction zone from relative positions in the reaction zone to carry out a contact reaction; the reaction product downwardly enters the solvent separation system and, under the action of the hot air conveying device, enters the cyclone separation device; after separation, the solvent enters the solvent recovery system to achieve separation and recovery; the reaction product enters the lower discharge port of the cyclone separation device to obtain a polyurea thickener powder; In step S1, the preheating temperature of the reaction zone is 50-70°C, and the preheating temperature of the separation zone is 110-130°C; In step S2, the amine is one or more of aliphatic amines and aromatic amines; the isocyanate is one of monoisocyanate, diisocyanate or polyisocyanate; The solvent is a low-boiling point base oil or an organic solvent; The total weight of the amine and the isocyanate is 10% to 85% of the total weight of the solvent.

2. The method for preparing polyurea thickener powder according to claim 1, characterized in that: The hot air conveying device includes a blower and a heating device; And / or, the solvent separation system further comprises a collection tank disposed below the cyclone separation device for collecting the polyurea thickener powder.

3. The method for preparing polyurea thickener powder according to claim 2, characterized in that: An amine liquid booster pump is provided between the amine dissolving tank and the amine liquid spraying device; an isocyanate booster pump is provided between the isocyanate dissolving tank and the isocyanate spraying device; The pressure adjustment range of the amine liquid booster pump and the isocyanate booster pump is 0~1MPa.

4. The method for preparing polyurea thickener powder according to claim 3, characterized in that: The solvent recovery system includes a solvent collecting device and a condensing device; The solvent collection device includes a solvent flow area, a solvent recovery area and a solvent condensation area; the solvent flow area is sealed and connected to the top of the cyclone separation device; the solvent recovery area is vertically connected to the solvent flow area; the solvent condensation area is vertically connected to the solvent recovery area, and a solvent outlet is provided at the bottom of the solvent condensation area; the condensation device is arranged in the solvent condensation area.

5. The method for preparing polyurea thickener powder according to claim 4, characterized in that: A temperature sensor is provided on the top of the solvent collecting device; And / or, the condensing medium of the condensing device includes cooling water or chilled brine; the flow direction of the condensing medium is opposite to the outflow direction of the solvent.

6. The method for preparing the polyurea thickener powder according to any one of claims 1 to 5, characterized in that: In step S2, the amine is one or more of octylamine, dodecylamine, hexadecylamine, octadecylamine, aniline, p-toluidine, cyclohexylamine, dicyclohexylamine, p-chloroaniline, m-phenylenediamine, p-phenylenediamine, o-phenylenediamine, melamine, dibenzimidazole diamine, and benzidine; The isocyanate is one or more of toluene diisocyanate, isophorone diisocyanate, diphenylmethane diisocyanate, dicyclohexylmethane diisocyanate, hexamethylene diisocyanate, and lysine diisocyanate; The solvent is one or more of ethyl acetate, toluene, acetone, chloroform, benzene and petroleum ether.

Citation Information

Patent Citations

  • High-dropping-point lubricating grease and prefabricated soap making method

    CN100378209C

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