Method and apparatus for coagulation of rubber polymers

Abstract

The invention relates to the field of synthetic rubber, and discloses a method and a device for rubber polymer coagulation. The method comprises the following steps: filtering a rubber polymer solution by adopting a water pressure filter, carrying out first contact on the obtained rubber solution, condensed water and steam I, and separating the material after the first contact to obtain water I and first rubber particle water; performing second contact on the first colloidal particle water and steam II, and separating the material after the second contact to obtain water II and second colloidal particle water; concentrating the second colloidal particle water to obtain water III and third colloidal particle water; performing third contact on the third colloidal particle water and the steam III, and separating the material after the third contact to obtain water IV and fourth colloidal particle water; circulating a first part of water III as reuse water through a first booster pump for first contact; the amount of the reuse water is 15-40% of the total water amount by volume. The method can reduce the consumption of steam and solvent, and is lower in cost, stable in return water consumption, long in operation cycle and high in device utilization rate.

Description

Technical Field

[0001] The present invention relates to the field of synthetic rubber, and particularly to a method and a device for rubber polymer coagulation. Background Art

[0002] Currently, most domestic solution polymerization rubber plants adopt the three-kettle coagulation process by water precipitation method. With the continuous improvement of environmental protection and energy conservation requirements, developing a new and energy-saving coagulation process to further reduce energy consumption, material consumption, reduce the discharge of three wastes, and reduce costs has become a hot research topic in this field.

[0003] CN107793504A discloses a device for rubber polymer coagulation. This device adopts a process technology combining three-kettle differential pressure coagulation and rubber particle concentration enhancement technology. Between the first coagulation kettle and the second coagulation kettle, and between the second coagulation kettle and the third coagulation kettle, a water distribution pipe is installed for concentration enhancement. Through two times of concentration enhancement, energy conservation and consumption reduction are achieved. Although the process flow of this device is simple and convenient for maintenance, the filter screen is frequently blocked and the maintenance frequency is high, which is not conducive to the stable operation of the device.

[0004] CN102382214A discloses a coagulation process for the production of polymerization products. This coagulation process combines the three-kettle differential pressure coagulation process with the rubber particle concentration enhancement technology to alleviate the contradiction between energy conservation and consumption reduction, achieving the purpose of reducing solvent consumption and steam usage. However, this method only recycles part of the high-temperature hot water in the second coagulation, and the recycled water volume is low, and the energy-saving effect is not obvious. Secondly, the high-temperature recycled hot water recycled by its concentrator is unstable. It is necessary to close the pipeline valve from the second coagulation kettle to the third coagulation kettle to adjust the recycled water volume, which is not convenient to operate and is prone to block the pipeline.

[0005] CN102516419A discloses a three-kettle coagulation method in the production of synthetic rubber by solution polymerization method. This method solves the problems of high steam consumption and high solvent residue content in the two-kettle coagulation process. Although this method has made great progress in energy conservation and consumption reduction of three-kettle coagulation, the pressure control of its first coagulation kettle is relatively low, and the gas phases of the second and third coagulation kettles all enter the first coagulation kettle, resulting in low heat utilization rate and relatively high steam consumption. Summary of the Invention

[0006] The object of the present invention is to overcome the problems existing in the prior art, such as the coagulation pipeline is easy to be blocked, difficult to maintain, the recycled water volume is unstable, and the consumption of steam and solvent is large.

[0007] To achieve the above object, in the first aspect of the present invention, a method for rubber polymer coagulation is provided, and the method includes:

[0008] (1) Filter the rubber polymer solution using a hydraulic pressure filter, then bring the filtered glue solution into first contact with condensed water and steam I, and separate the material after the first contact to obtain water I and first colloidal particle water;

[0009] (2) Bring the first colloidal particle water into second contact with steam II, and separate the material after the second contact to obtain water II and second colloidal particle water; Concentrate the second colloidal particle water to obtain water III and third colloidal particle water;

[0010] (3) Bring the third colloidal particle water into third contact with steam III, and separate the material after the third contact to obtain water IV and fourth colloidal particle water;

[0011] Among them, a first part of the water III in step (2) is recycled as recycled water to step (1) through a first booster pump for the first contact; the amount of the recycled water is 15 - 40% by volume of the total water volume.

[0012] A second aspect of the present invention provides a device for rubber polymer coagulation. The device includes a hydraulic pressure filter, a first coagulation kettle, a second coagulation kettle, and a third coagulation kettle connected in series in sequence; wherein:

[0013] A first concentrator is provided between the second coagulation kettle and the third coagulation kettle. The inlet of the first concentrator is communicated with the colloidal particle water outlet of the second coagulation kettle, the concentrated colloidal particle water outlet of the first concentrator is communicated with the inlet of the third coagulation kettle, and the concentrated water outlet of the first concentrator is communicated with the inlet of the first coagulation kettle; A first booster pump is also provided between the first concentrator and the first coagulation kettle.

[0014] Through the above technical solutions, the method and device provided by the present invention have the following advantages:

[0015] (1) Adopt pressurized power transmission and flow control, that is, use a pump to transport colloidal particle water, especially use a booster pump to transport recycled water, which strengthens the flow state of the fluid, changes from the mainly laminar flow of traditional overflow transmission to the mainly turbulent flow of power transmission, reduces the blockage caused by colloidal particles sticking to the pipe wall, the amount of recycled water can reach 15 - 40% by volume of the total water volume, and at the same time can ensure that the content of suspended solids in the recycled water is below 0.5 g / 100 g, and ensures the stability of the recycled water volume;

[0016] (2) Using a water-washed hydraulic pressure filter can effectively improve the solvent recovery rate, reduce the emission of VOCs during the production process of synthetic rubber, reduce solvent consumption while reducing carbon emissions, and is beneficial to environmental protection;

[0017] (3) Preferably, four - kettle coagulation is adopted to extend the residence time of the rubber particles in the low - pressure area of the coagulation kettle, effectively reducing the solvent content in the rubber, as well as the solvent consumption of the coagulation system and the carbon emissions of the post - treatment. In addition, combined with the three - kettle coagulation and / or four - kettle coagulation with concentration enhancement treatment, not only can the residence time of the rubber particles be effectively extended, but also the solvent recovery rate can be increased, the oil content in the synthetic rubber can be reduced, and the solvent consumption is small.

[0018] (4) Preferably, by using the heat of the gas phase in the second coagulation kettle, the third coagulation kettle, and the fourth coagulation kettle, the loss of the gas - phase heat is effectively reduced. By recycling the high - temperature hot water from the second coagulation kettle, the third coagulation kettle, and the fourth kettle, more than 50% of the high - temperature hot water in the coagulation system is recycled, effectively reducing the loss of the liquid - phase heat, reducing the steam consumption of the coagulation system, and achieving better energy - saving effects.

[0019] (5) Preferably, a water - washing hydraulic filter is adopted, and the back - washing water of the concentration enhancer is used to wash and replace the hydraulic filter, and all the solvents in the polymer solution are separated and sent to the coagulation kettle for recycling, effectively reducing the solvent consumption and at the same time reducing the carbon emissions.

[0020] In summary, the device and method provided by the present invention can achieve the energy - saving effect of reducing steam consumption and the consumption - reduction effect of reducing solvent consumption, with lower costs, stable back - water usage, long operation cycles, and can also improve the utilization rate of the device. Description of the Drawings

[0021] Figure 1 is a schematic process flow diagram for rubber polymer coagulation according to an embodiment of the present invention;

[0022] Figure 2 is a schematic process flow diagram for rubber polymer coagulation according to an embodiment of the present invention;

[0023] Figure 3 is a schematic process flow diagram for rubber polymer coagulation according to an embodiment of the present invention.

[0024] Description of the Reference Numerals

[0025] 1. Sprayed hot water 2. Rubber solution 3. Steam 4. Post - treatment unit

[0026] 5. Steam for air extractor 6. Steam for air extractor 7. Steam for back - flushing 8. Hot water for back - flushing 9. Hydraulic filter 10. Rubber tank 11. Solvent oil 12. Cooler 13. Water - cooled cooler 14. Oil - water separation tank 15. Oil tank

[0027] F1, the first coagulation kettle; F2, the second coagulation kettle; F3, the third coagulation kettle; F4, the fourth coagulation kettle; P1, the first inter-kettle pump; P2, the second inter-kettle pump; P3, the third inter-kettle pump; P4, the fourth inter-kettle pump; P5, the spray glue pump; P6, the second booster pump; P7, the seventh inter-kettle pump

[0028] T1, the first concentration enhancer; T2, the second concentration enhancer; T3, the third concentration enhancer

[0029] W1, the first steam ejector; W2, the second steam ejector Detailed implementation manners

[0030] In the ranges disclosed herein, the endpoints and any values of the ranges are not limited to the exact ranges or values. These ranges or values should be understood to include values close to these ranges or values. For numerical ranges, between the endpoint values of each range, between the endpoint values of each range and individual point values, and between individual point values, they can be combined with each other to obtain one or more new numerical ranges, and these numerical ranges should be regarded as specifically disclosed herein.

[0031] In the present invention, unless otherwise specified, the "first", "second", "third", etc. and the serial numbers such as "I", "II", "III", etc. in the names of each material and each operation name do not represent the order of priority, nor do they limit each material or operation. They are only used to distinguish each material or operation. For example, the "first", "second", "third", etc. in "the first rubber particle water", "the second rubber particle water", "the third rubber particle water", etc. are only used to distinguish to indicate that this is not the same rubber particle water; the "water I", "water II", "water III", etc. are only used to distinguish to indicate that this is not the same product; the "first contact", "second contact", "third contact", etc. are only used to distinguish to indicate that this is not the same contact reaction operation. The definitions of the serial numbers in the names of the remaining materials and operation names are similar and will not be elaborated here.

[0032] As described above, the first aspect of the present invention provides a method for coagulating a rubber polymer, and the method includes:

[0033] (1) Filter the rubber polymer solution using a hydraulic filter, and then make the first contact of the filtered glue solution with coagulation water and steam I, and separate the materials after the first contact to obtain water I and the first rubber particle water;

[0034] (2) Make the second contact of the first rubber particle water with steam II, and separate the materials after the second contact to obtain water II and the second rubber particle water; subject the second rubber particle water to concentration treatment to obtain water III and the third rubber particle water;

[0035] (3) Bring the third colloidal particle water into third contact with steam III, and separate the material after the third contact to obtain water IV and fourth colloidal particle water;

[0036] Wherein, a first part of the water III in step (2) is recycled as recycled water to step (1) through a first booster pump for the first contact; the amount of the recycled water is 15-40% by volume of the total water volume.

[0037] According to some embodiments of the present invention, a first part of the water III in step (2) is recycled as recycled water to step (1) through a first booster pump for the first contact. By using a booster pump, the stability of the recycled water amount can be ensured, and the method has a long operation cycle. In addition, the use of recycled water reduces the heat loss of hot water in post-treatment flashing and reduces the steam consumption of the first contact. The amount of the recycled water is 15-40% by volume of the total water volume. The density of the colloidal particle water in the third coagulation kettle is increased by nearly 17.5-67.5% compared with that in the second coagulation kettle, effectively increasing the coagulation time in the third coagulation kettle by 0.17-0.42 h, improving the coagulation effect, reducing the oil content in the rubber, and reducing the steam consumption by 0.36-0.8 t.

[0038] According to some embodiments of the present invention, preferably, in step (1), the conditions of the first contact include: gauge pressure is 0.06-0.08 MPa, and temperature is 85-95 °C.

[0039] According to some embodiments of the present invention, preferably, in step (2), the conditions of the second contact include: gauge pressure is 0.03-0.05 MPa, and temperature is 100-105 °C.

[0040] According to some embodiments of the present invention, preferably, in step (3), the conditions of the third contact include: gauge pressure is 0-0.02 MPa, and temperature is 95-100 °C.

[0041] According to some embodiments of the present invention, preferably, the rubber polymer solution is at least one of a nickel-based cis-1,4-polybutadiene rubber solution, a rare earth cis-1,4-polybutadiene rubber solution, a rare earth isoprene rubber solution, and a styrene-butadiene rubber solution; the solvent in the rubber polymer solution is hexane and / or cyclohexane; in the rubber polymer solution, the content of the rubber polymer is 15-20% by weight.

[0042] According to some embodiments of the present invention, preferably, the second part of the water III in step (2) is recycled as a cleaning liquid to step (1) to clean the pressure filter, and the cleaning liquid after cleaning is used as condensate water for the first contact. The sum of the first part and the second part of the water III is the water III. By adopting the above preferred embodiment, the solution in the glue liquid in the pressure filter is completely recovered into the coagulation kettle, and the subsequent cleaning operation is carried out using the filter after cleaning, without VOC emission, avoiding environmental pollution, and at the same time reducing the solvent consumption in the coagulation process.

[0043] According to some embodiments of the present invention, preferably, at least one of the water I, the water II, and the water IV is recycled as coagulation water to step (1) for the first contact.

[0044] According to some embodiments of the present invention, preferably, the gas phase separated in step (3) is returned to step (2) for the second contact.

[0045] According to some embodiments of the present invention, preferably, the gas phase separated in step (2) is returned to step (1) for the first contact.

[0046] By adopting the above preferred embodiment, the heat of the separated high-temperature gas phase is further utilized, reducing the steam consumption in the first contact and the second contact, and reducing the gas-phase refrigerant consumption in the second contact and the third contact, which is beneficial to waste heat recovery and energy conservation, thereby further reducing the steam consumption and making the method more energy-efficient.

[0047] According to some embodiments of the present invention, preferably, step (1) further includes: concentrating the first colloidal particle water to obtain concentrated water and concentrated colloidal particle water, and carrying out the second contact between the concentrated colloidal particle water and the steam II in step (2).

[0048] According to some embodiments of the present invention, preferably, the method further includes: concentrating the fourth colloidal particle water in step (3) to obtain water V and fifth colloidal particle water.

[0049] According to some embodiments of the present invention, preferably, the method further includes: circulating the first part of the water V as recycled water to step (2) through a second booster pump for the second contact; the amount of the recycled water is 10-20% by volume of the total water volume. By adopting the above preferred embodiment, it is beneficial to further reduce the steam consumption.

[0050] According to some embodiments of the present invention, preferably, the second part of the water V is recycled to step (1) for the first contact. The sum of the first part and the second part of the water V is the water V.

[0051] According to some embodiments of the present invention, preferably, the method further includes: subjecting the fourth colloidal particle water in step (3) to a fourth contact with steam IV, and separating the material after the fourth contact to obtain water VI and sixth colloidal particle water. By adopting the above preferred embodiments, it is beneficial to further extend the residence time of the colloidal particles and further reduce the consumption of the solvent.

[0052] According to some embodiments of the present invention, preferably, the method further includes: concentrating the sixth colloidal particle water to obtain water VII and seventh colloidal particle water; circulating the first part of the water VII as recycled water to step (2) through a second booster pump for the second contact; the amount of the recycled water is 10-20% by volume of the total water volume.

[0053] According to some embodiments of the present invention, preferably, the conditions of the fourth contact include: gauge pressure of 0-0.02 MPa and temperature of 95-100 °C.

[0054] According to some embodiments of the present invention, preferably, the separated gas phase is returned to step (2) for the second contact. By adopting the above preferred embodiments, the heat of the separated high-temperature gas phase is further utilized, reducing the steam consumption in the first contact and the second contact, and reducing the gas-phase refrigerant consumption in the second contact, the third contact and the fourth contact, which is beneficial to recovering waste heat and saving energy, thereby further reducing the steam consumption and making the method more energy-efficient.

[0055] According to some embodiments of the present invention, preferably, the second part of the water VI and / or the water VII is recycled to step (1) for the first contact. The sum of the first part and the second part of the water VII is the water VII.

[0056] In the method according to some embodiments of the present invention, different contact operations remove the solvent in different ways. Among them, the saturated steam pressure of the first contact is relatively high. Therefore, preferably, the energy consumption is reduced by lowering the operating temperature and increasing the pressure; the vapor pressure of the second contact is relatively low, and a higher temperature is required to remove the solvent. Therefore, preferably, the solvent is removed by lowering the pressure and increasing the operating temperature to reduce the solvent consumption; in the third contact and the fourth contact, preferably, the residence time is extended and the pressure is controlled to be a lower slightly positive pressure to further separate the remaining solvent, and finally the purpose of solvent removal is achieved.

[0057] The second aspect of the present invention provides a device for rubber polymer coagulation, which includes a hydraulic filter, a first coagulation kettle, a second coagulation kettle, and a third coagulation kettle connected in series and in communication in sequence; wherein:

[0058] A first thickener is arranged between the second coagulation kettle and the third coagulation kettle. The inlet of the first thickener is communicated with the rubber particle water outlet of the second coagulation kettle, the concentrated rubber particle water outlet of the first thickener is communicated with the inlet of the third coagulation kettle, and the concentrated water outlet of the first thickener is communicated with the inlet of the first coagulation kettle; A first booster pump is also arranged between the first thickener and the first coagulation kettle.

[0059] In the existing coagulation device, the filter is an oil pressure filter (and the filter is cleaned with solvent oil); only a pipeline is used to connect the first thickener and the first coagulation kettle; and the steam outlet of the third coagulation kettle is communicated with the steam inlet in the middle of the first coagulation kettle through a steam ejector; the steam outlet of the second coagulation kettle is communicated with the steam inlet at the bottom of the first coagulation kettle. This device only relies on the inter-kettle pump for the transportation of materials, resulting in easy blockage of the coagulation pipeline, difficult maintenance, low and unstable water return volume, short operation cycle, and large consumption of steam and solvent. During the research process, the inventor of the present invention found that by using a booster pump to transport the recycled water, the flow state of the fluid is strengthened, changing from the laminar flow mainly of traditional overflow transportation to the turbulent flow mainly of power transportation, reducing the blockage caused by the rubber particles sticking to the pipe wall. The amount of recycled water can reach 15 - 40% by volume of the total water volume, and at the same time, it can ensure that the content of suspended solids in the recycled water is below 0.5 g / 100 g, and ensure the stability of the recycled water volume; at the same time, using a water-washed hydraulic filter can effectively improve the solvent recovery rate, reduce the emission of VOC during the production of synthetic rubber, reduce the solvent consumption and carbon emissions while playing a role, which is beneficial to environmental protection.

[0060] According to some embodiments of the present invention, preferably, a regulating valve and a flow meter are also arranged on the pipeline between the first booster pump and the first coagulation kettle to control the flow rate of the recycled water;

[0061] According to some embodiments of the present invention, preferably, the steam outlet of the third coagulation kettle is communicated with the inlet of the second coagulation kettle; a first steam ejector is also arranged between the steam outlet of the third coagulation kettle and the inlet of the second coagulation kettle. The first steam ejector can control the temperature in the second coagulation kettle.

[0062] According to some embodiments of the present invention, preferably, the steam outlet of the second coagulation kettle is communicated with the inlet of the first coagulation kettle; a second steam ejector is also arranged between the steam outlet of the second coagulation kettle and the inlet of the first coagulation kettle. The second steam ejector can control the temperature in the first coagulation kettle.

[0063] According to some embodiments of the present invention, preferably, the concentrated water outlet of the first concentration unit is communicated with the cleaning inlet of the hydraulic pressure filter; the cleaning outlet of the hydraulic pressure filter is communicated with the inlet of the first coagulation kettle.

[0064] According to some embodiments of the present invention, preferably, a cooler, a water cooler and an oil-water separation tank are sequentially arranged at the steam outlet of the first coagulation kettle to separate oil and water from the gas phase at the top of the first coagulation kettle, so as to recycle the solvent oil, and the recycled solvent oil can be stored in an oil tank.

[0065] According to some embodiments of the present invention, preferably, a second concentration unit is further arranged between the first coagulation kettle and the second coagulation kettle. The inlet of the second concentration unit is communicated with the colloidal particle water outlet of the first coagulation kettle, and the concentrated colloidal particle water outlet of the second concentration unit is communicated with the inlet of the second coagulation kettle.

[0066] According to some embodiments of the present invention, preferably, the concentrated water outlet of the second concentration unit is communicated with the post-treatment unit; a regulating valve and a flowmeter are further arranged on the pipeline between the concentrated water outlet of the second concentration unit and the post-treatment unit to control the flow rate of the concentrated water.

[0067] According to some embodiments of the present invention, preferably, a third concentration unit is further arranged at the colloidal particle water outlet of the third coagulation kettle. The inlet of the third concentration unit is communicated with the colloidal particle water outlet of the third coagulation kettle, and the concentrated water outlet of the third concentration unit is communicated with the inlet of the second coagulation kettle.

[0068] According to some embodiments of the present invention, preferably, a second booster pump is further arranged between the third concentration unit and the second coagulation kettle. Preferably, a regulating valve and a flowmeter are further arranged on the pipeline between the second booster pump and the second coagulation kettle to control the flow rate of the recycled water.

[0069] According to some embodiments of the present invention, preferably, the device further includes a fourth coagulation kettle, and the inlet of the fourth coagulation kettle is communicated with the colloidal particle water outlet of the third coagulation kettle.

[0070] Preferably, a third concentration unit is further arranged at the colloidal particle water outlet of the fourth coagulation kettle. The inlet of the third concentration unit is communicated with the colloidal particle water outlet of the fourth coagulation kettle, and the concentrated water outlet of the third concentration unit is communicated with the inlet of the second coagulation kettle.

[0071] Preferably, a second booster pump is further arranged between the third concentration unit and the second coagulation kettle.

[0072] Preferably, the steam outlet of the fourth coagulation kettle is communicated with the inlet of the first steam ejector.

[0073] According to some embodiments of the present invention, preferably, the device further includes an anti-purging pipeline for the concentrator and a water replenishing pipeline for the third coagulation kettle, which is beneficial to further avoid the situation that the glue density in the third coagulation kettle is too high, resulting in overload of the agitator motor and difficulty in transporting the glue particles in water.

[0074] The following will describe in detail the methods and devices provided by the present invention with reference to the accompanying drawings.

[0075] Figure 1 It is a schematic process flow diagram for rubber polymer coagulation according to an embodiment of the present invention. It can be seen from the figure that the device for rubber polymer coagulation includes a hydraulic filter 9, a first coagulation kettle F1, a second coagulation kettle F2, and a third coagulation kettle F3 connected in series and in communication in sequence; among them:

[0076] A first inter-kettle pump P1 is arranged between the first coagulation kettle F1 and the second coagulation kettle F2;

[0077] A first concentrator T1 is arranged between the second coagulation kettle F2 and the third coagulation kettle F3. The inlet of the first concentrator T1 is communicated with the glue particle water outlet of the second coagulation kettle F2; a second inter-kettle pump P2 is also arranged between the inlet of the first concentrator T1 and the glue particle water outlet of the second coagulation kettle F2; the concentrated glue particle water outlet of the first concentrator T1 is communicated with the inlet of the third coagulation kettle F3, and the concentrated water outlet of the first concentrator T1 is communicated with the inlet of the first coagulation kettle F1; a first booster pump P4 is also arranged between the first concentrator T1 and the first coagulation kettle F1; a regulating valve and a flow meter are also arranged on the pipeline between the first booster pump P4 and the first coagulation kettle F1;

[0078] The glue particle water outlet of the third coagulation kettle F3 is communicated with the post-treatment unit 4 through a third inter-kettle pump P3;

[0079] The steam outlet of the third coagulation kettle F3 is communicated with the steam inlet in the middle of the second coagulation kettle F2; a first steam ejector W1 is also arranged between the steam outlet of the third coagulation kettle F3 and the steam inlet in the middle of the second coagulation kettle F2; the steam outlet of the second coagulation kettle F2 is communicated with the steam inlet in the middle of the first coagulation kettle F1; a second steam ejector W2 is also arranged between the steam outlet of the second coagulation kettle F2 and the steam inlet in the middle of the first coagulation kettle F1;

[0080] The concentrated water outlet of the first concentrator T1 is communicated with the cleaning inlet of the hydraulic filter 9; the cleaning outlet of the hydraulic filter 9 is communicated with the inlet of the first coagulation kettle F1;

[0081] The steam outlet of the first coagulation kettle F1 is successively provided with a cooler 12, a water cooler 13, an oil-water separation tank 14 and an oil tank 15;

[0082] The device further includes a rubber polymer solution storage tank 10, and the rubber polymer solution storage tank 10 is communicated with the inlet of the water pressure filter 9 through a glue spraying pump P5.

[0083] The method for rubber polymer coagulation includes:

[0084] (1) Filter the rubber polymer solution from the rubber polymer solution storage tank 10 by using a water pressure filter 9, and then in the first coagulation kettle F1, make the filtered glue liquid 2 contact with coagulation water and steam I for the first time, and separate the material after the first contact to obtain water I and first colloidal particle water, and send the first colloidal particle water to the second coagulation kettle F2 through a first inter-kettle pump P1;

[0085] Wherein, the coagulation water includes the sprayed hot water 1 from the post-treatment unit 4;

[0086] (2) In the second coagulation kettle F2, make the first colloidal particle water contact with steam II for the second time, and separate the material after the second contact to obtain water II and second colloidal particle water;

[0087] Send the second colloidal particle water to the first thickener T1 through a second inter-kettle pump P2 for thickening treatment to obtain water III and third colloidal particle water, and send the third colloidal particle water to the third coagulation kettle F3;

[0088] Circulate a first part of the water III to the first coagulation kettle F1 in step (1) as recycled water through a first booster pump P4 for the first contact;

[0089] (3) In the third coagulation kettle F3, make the third colloidal particle water contact with steam III for the third time, and separate the material after the third contact to obtain water IV and fourth colloidal particle water;

[0090] Send the fourth colloidal particle water to the post-treatment unit 4 through a third inter-kettle pump P3;

[0091] Wherein, the steam I and the steam II are provided by steam 3; the steam III is provided by backwashing steam 7; backwash the first thickener T1 with backwashing steam 7 and / or backwashing hot water 8;

[0092] Send the gas phase separated in step (3) (the gas phase at the top of the third coagulation kettle F3) back to the middle of the second coagulation kettle F2 through a first steam ejector W1 along with the air extractor steam 6 for the second contact;

[0093] The gas phase separated in step (2) (the gas phase at the top of the second coagulation kettle F2) is returned to the middle of the first coagulation kettle F1 through the second steam ejector W2 with the steam ejector using steam 5 for the first contact;

[0094] The second part of the water III in step (2) is circulated as a cleaning liquid to step (1) to clean the hydraulic pressure filter 9, and the cleaned cleaning liquid is sent to the first coagulation kettle F1 as coagulated water for the first contact;

[0095] At least one of the water I, the water II, and the water IV is circulated as coagulated water to the first coagulation kettle F1 in step (1) for the first contact;

[0096] The gas phase separated in step (1) (the gas phase at the top of the first coagulation kettle F1) enters the oil-water separation tank 14 through the cooler 12 and the water cooler 13 in sequence for oil-water separation to recycle the solvent oil 11 for reuse, and the recycled solvent oil 11 is stored in the oil tank 15.

[0097] Figure 2 It is a schematic process flow diagram of a rubber polymer coagulation method according to an embodiment of the present invention. It can be seen from the figure that the device for rubber polymer coagulation includes a hydraulic pressure filter 9, a first coagulation kettle F1, a second coagulation kettle F2, and a third coagulation kettle F3 connected in series in sequence; wherein:

[0098] A first inter-kettle pump P1 and a second concentration enhancer T2 are arranged in sequence between the first coagulation kettle F1 and the second coagulation kettle F2; the inlet of the second concentration enhancer T2 is connected to the rubber particle water outlet of the first coagulation kettle F1 through the first inter-kettle pump P1, and the concentrated rubber particle water outlet of the second concentration enhancer T2 is connected to the inlet of the second coagulation kettle F2; the concentrated water outlet of the second concentration enhancer T2 is connected to the post-treatment unit 4; a regulating valve and a flow meter are also arranged on the pipeline between the concentrated water outlet of the second concentration enhancer T2 and the post-treatment unit 4;

[0099] A first concentration enhancer T1 is arranged between the second coagulation kettle F2 and the third coagulation kettle F3, and the inlet of the first concentration enhancer T1 is connected to the rubber particle water outlet of the second coagulation kettle F2; a second inter-kettle pump P2 is also arranged between the inlet of the first concentration enhancer T1 and the rubber particle water outlet of the second coagulation kettle F2; the concentrated rubber particle water outlet of the first concentration enhancer T1 is connected to the inlet of the third coagulation kettle F3, and the concentrated water outlet of the first concentration enhancer T1 is connected to the inlet of the first coagulation kettle F1; a first booster pump P4 is also arranged between the first concentration enhancer T1 and the first coagulation kettle F1; a regulating valve and a flow meter are also arranged on the pipeline between the first booster pump P4 and the first coagulation kettle F1;

[0100] A third thickener T3 is also provided at the colloidal particle water outlet of the third coagulation kettle F3. The inlet of the third thickener T3 is communicated with the colloidal particle water outlet of the third coagulation kettle F3 via a third inter-kettle pump P3, and the thickened water outlet of the third thickener T3 is communicated with the inlet of the second coagulation kettle F2;

[0101] The thickened colloidal particle water outlet of the third thickener T3 is communicated with the post-treatment unit 4; A second booster pump P6 is also provided between the third thickener T3 and the second coagulation kettle F2; A regulating valve and a flow meter are also provided on the pipeline between the second booster pump P6 and the second coagulation kettle F2;

[0102] The steam outlet of the third coagulation kettle F3 is communicated with the steam inlet in the middle of the second coagulation kettle F2; A first steam ejector W1 is also provided between the steam outlet of the third coagulation kettle F3 and the steam inlet in the middle of the second coagulation kettle F2; The steam outlet of the second coagulation kettle F2 is communicated with the steam inlet in the middle of the first coagulation kettle F1; A second steam ejector W2 is also provided between the steam outlet of the second coagulation kettle F2 and the steam inlet in the middle of the first coagulation kettle F1;

[0103] The thickened water outlet of the first thickener T1 is communicated with the cleaning inlet of the hydraulic pressure filter 9; The cleaning outlet of the hydraulic pressure filter 9 is communicated with the inlet of the first coagulation kettle F1;

[0104] A cooler 12, a water cooler 13, an oil-water separation tank 14 and an oil tank 15 are successively provided at the steam outlet of the first coagulation kettle F1;

[0105] The device also includes a rubber polymer solution storage tank 10, and the rubber polymer solution storage tank 10 is communicated with the inlet of the hydraulic pressure filter 9 via a glue spraying pump P5.

[0106] The method for rubber polymer coagulation includes:

[0107] (1) Filter the rubber polymer solution from the rubber polymer solution storage tank 10 using the hydraulic pressure filter 9, and then in the first coagulation kettle F1, bring the filtered glue liquid 2 into first contact with coagulation water and steam I, and separate the material after the first contact to obtain water I and first colloidal particle water;

[0108] Among them, the coagulation water includes the sprayed hot water 1 from the post-treatment unit 4;

[0109] Send the first colloidal particle water to the second thickener T2 via the first inter-kettle pump P1 for thickening treatment to obtain thickened water and thickened colloidal particle water, send the thickened water to the post-treatment unit 4; Send the thickened colloidal particle water to the second coagulation kettle F2;

[0110] (2) In the second agglomeration kettle F2, the concentrated colloidal particle water is brought into second contact with steam II, and the material after the second contact is separated to obtain water II and second colloidal particle water;

[0111] The second colloidal particle water is sent to the first concentrator T1 through the second inter-kettle pump P2 for concentration treatment to obtain water III and third colloidal particle water, and the third colloidal particle water is sent to the third agglomeration kettle F3;

[0112] A first part of the water III is recycled as recycled water to the first agglomeration kettle F1 in step (1) through the first booster pump P4 for the first contact;

[0113] (3) In the third agglomeration kettle F3, the third colloidal particle water is brought into third contact with steam III, and the material after the third contact is separated to obtain water IV and fourth colloidal particle water;

[0114] The fourth colloidal particle water is sent to the third concentrator T3 through the third inter-kettle pump P3 for concentration treatment to obtain water V and fifth colloidal particle water;

[0115] A first part of the water V is recycled as recycled water to step (2) through the second booster pump P6 for the second contact; the fifth colloidal particle water is sent to the post-treatment unit 4; a second part of the water V is recycled to step (1) for the first contact;

[0116] Among them, the steam I and the steam II are provided by steam 3; the steam III is provided by the backwashing steam 7; the first concentrator T1 is backwashed by the backwashing steam 7 and / or the backwashing hot water 8;

[0117] The gas phase separated in step (3) (the top gas phase of the third agglomeration kettle F3) is returned to the middle part of the second agglomeration kettle F2 through the first steam ejector W1 along with the air extractor steam 6 for the second contact;

[0118] The gas phase separated in step (2) (the top gas phase of the second agglomeration kettle F2) is returned to the middle part of the first agglomeration kettle F1 through the second steam ejector W2 along with the air extractor steam 5 for the first contact;

[0119] A second part of the water III in step (2) is recycled as a cleaning liquid to step (1) to clean the water pressure filter 9, and the cleaning liquid after cleaning is sent to the first agglomeration kettle F1 as agglomerated water for the first contact;

[0120] At least one of the water I, the water II, and the water IV is recycled as agglomerated water to the first agglomeration kettle F1 in step (1) for the first contact;

[0121] The gaseous phase separated in step (1) (the gaseous phase at the top of the first coagulation kettle F1) is successively passed through a cooler 12 and a water cooler 13 and then enters an oil-water separation tank 14 for oil-water separation to recover the solvent oil 11 for recycling. The recovered solvent oil 11 is stored in an oil tank 15.

[0122] Figure 3 It is a schematic process flow diagram of a rubber polymer coagulation method according to an embodiment of the present invention. As can be seen from the figure, the device for rubber polymer coagulation includes a hydraulic filter 9, a first coagulation kettle F1, a second coagulation kettle F2, a third coagulation kettle F3, and a fourth coagulation kettle F4 that are connected in series in sequence; where:

[0123] A first inter-kettle pump P1 and a second concentrator T2 are successively arranged between the first coagulation kettle F1 and the second coagulation kettle F2; the inlet of the second concentrator T2 is connected to the rubber particle water outlet of the first coagulation kettle F1 through the first inter-kettle pump P1, and the concentrated rubber particle water outlet of the second concentrator T2 is connected to the inlet of the second coagulation kettle F2; the concentrated water outlet of the second concentrator T2 is connected to a post-treatment unit 4; a regulating valve and a flowmeter are also arranged on the pipeline between the concentrated water outlet of the second concentrator T2 and the post-treatment unit 4;

[0124] A first concentrator T1 is arranged between the second coagulation kettle F2 and the third coagulation kettle F3, and the inlet of the first concentrator T1 is connected to the rubber particle water outlet of the second coagulation kettle F2; a second inter-kettle pump P2 is also arranged between the inlet of the first concentrator T1 and the rubber particle water outlet of the second coagulation kettle F2; the concentrated rubber particle water outlet of the first concentrator T1 is connected to the inlet of the third coagulation kettle F3, and the concentrated water outlet of the first concentrator T1 is connected to the inlet of the first coagulation kettle F1; a first booster pump P4 is also arranged between the first concentrator T1 and the first coagulation kettle F1; a regulating valve and a flowmeter are also arranged on the pipeline between the first booster pump P4 and the first coagulation kettle F1;

[0125] The inlet of the fourth coagulation kettle F4 is connected to the rubber particle water outlet of the third coagulation kettle F3 through a third inter-kettle pump P3;

[0126] A third concentrator T3 is also arranged at the rubber particle water outlet of the fourth coagulation kettle F4. The inlet of the third concentrator T3 is connected to the rubber particle water outlet of the fourth coagulation kettle F4 through a fourth inter-kettle pump P7, and the concentrated water outlet of the third concentrator T3 is connected to the inlet of the second coagulation kettle F2;

[0127] The concentrated colloidal particle water outlet of the third concentration device T3 is communicated with the post-treatment unit 4; a second booster pump P6 is further arranged between the third concentration device T3 and the second coagulation kettle F2; a regulating valve and a flowmeter are further arranged on the pipeline between the second booster pump P6 and the second coagulation kettle F2;

[0128] The steam outlet of the third coagulation kettle F3 is communicated with the steam inlet in the middle of the second coagulation kettle F2; a first steam ejector W1 is further arranged between the steam outlet of the third coagulation kettle F3 and the steam inlet in the middle of the second coagulation kettle F2; the steam outlet of the second coagulation kettle F2 is communicated with the steam inlet in the middle of the first coagulation kettle F1; a second steam ejector W2 is further arranged between the steam outlet of the second coagulation kettle F2 and the steam inlet in the middle of the first coagulation kettle F1;

[0129] The steam outlet of the fourth coagulation kettle F4 is communicated with the inlet of the first steam ejector W1;

[0130] The concentrated water outlet of the first concentration device T1 is communicated with the cleaning inlet of the hydraulic pressure filter 9; the cleaning outlet of the hydraulic pressure filter 9 is communicated with the inlet of the first coagulation kettle F1;

[0131] A cooler 12, a water cooler 13, an oil-water separation tank 14 and an oil tank 15 are successively arranged at the steam outlet of the first coagulation kettle F1;

[0132] The device further includes a rubber polymer solution storage tank 10, and the rubber polymer solution storage tank 10 is communicated with the inlet of the hydraulic pressure filter 9 through a glue spraying pump P5.

[0133] The method for rubber polymer coagulation includes:

[0134] (1) Filter the rubber polymer solution from the rubber polymer solution storage tank 10 by using the hydraulic pressure filter 9, and then in the first coagulation kettle F1, make the filtered glue liquid 2 have a first contact with coagulation water and steam I, and separate the material after the first contact to obtain water I and first colloidal particle water;

[0135] Wherein, the coagulation water includes the sprayed hot water 1 from the post-treatment unit 4;

[0136] Send the first colloidal particle water to the second concentration device T2 through the first inter-kettle pump P1 for concentration treatment to obtain concentrated water and concentrated colloidal particle water, send the concentrated water to the post-treatment unit 4; send the concentrated colloidal particle water to the second coagulation kettle F2;

[0137] (2) In the second coagulation kettle F2, make the concentrated colloidal particle water have a second contact with steam II, and separate the material after the second contact to obtain water II and second colloidal particle water;

[0138] The second colloidal particle water is sent to a first concentrator T1 through a second between-kettle pump P2 for concentration treatment to obtain water III and third colloidal particle water, and the third colloidal particle water is sent to a third coagulation kettle F3;

[0139] A first part of the water III is recycled as recycled water to the first coagulation kettle F1 in step (1) through a first booster pump P4 for the first contact;

[0140] (3) In the third coagulation kettle F3, the third colloidal particle water is brought into third contact with steam III, and the material after the third contact is separated to obtain water IV and fourth colloidal particle water; the fourth colloidal particle water is sent to a fourth coagulation kettle F4 through a third between-kettle pump P3;

[0141] (4) In the fourth coagulation kettle F4, the fourth colloidal particle water is brought into fourth contact with steam IV, and the material after the fourth contact is separated to obtain water VI and sixth colloidal particle water;

[0142] The sixth colloidal particle water is sent to a third concentrator T3 through a fourth between-kettle pump P7 for concentration treatment to obtain water VII and seventh colloidal particle water;

[0143] A first part of the water VII is recycled as recycled water to step (2) through a second booster pump P6 for the second contact; the seventh colloidal particle water is sent to a post-treatment unit 4; a second part of the water VI and / or the water VII is recycled to step (1) for the first contact;

[0144] Among them, the steam I and the steam II are provided by steam 3; the steam III and the steam IV are provided by backwashing steam 7; the first concentrator T1 is backwashed by the backwashing steam 7 and / or backwashing hot water 8;

[0145] The gas phase separated in step (4) (the gas phase at the top of the fourth coagulation kettle F4) and the gas phase separated in step (3) (the gas phase at the top of the third coagulation kettle F3) are returned to the middle of the second coagulation kettle F2 through a first steam ejector W1 along with the steam for air extractor 6 for the second contact;

[0146] The gas phase separated in step (2) (the gas phase at the top of the second coagulation kettle F2) is returned to the middle of the first coagulation kettle F1 through a second steam ejector W2 along with the steam for air extractor 5 for the first contact;

[0147] A second part of the water III in step (2) is recycled as a cleaning liquid to step (1) to clean the pressure filter 9, and the cleaning liquid after cleaning is sent to the first coagulation kettle F1 as coagulated water for the first contact;

[0148] At least one of the water I, the water II, and the water IV is recycled as the coagulation water to the first coagulation kettle F1 in step (1) for the first contact.

[0149] The gas phase separated in step (1) (the gas phase at the top of the first coagulation kettle F1) enters the oil-water separation tank 14 through the cooler 12 and the water cooler 13 in sequence for oil-water separation, so as to recycle the solvent oil 11 for reuse, and the recycled solvent oil 11 is stored in the oil tank 15.

[0150] The present invention will be described in detail below through embodiments.

[0151] Embodiment 1

[0152] Adopt the device as Figure 1 shown to carry out the coagulation of the rubber polymer, and the specific method is as follows:

[0153] (1) Use the hydraulic filter 9 to filter the rubber polymer solution from the rubber tank 10, and then in the first coagulation kettle F1, make the filtered rubber solution 2 have the first contact with the coagulation water and the steam I, and separate the material after the first contact to obtain water I and the first colloidal particle water; send the first colloidal particle water to the second coagulation kettle F2 through the first inter-kettle pump P1;

[0154] Among them, the rubber polymer solution is a nickel-based cis-butadiene rubber solution (the content of the rubber polymer is 15% by weight), and the coagulation water includes the spray hot water 1 from the post-treatment unit 4;

[0155] The conditions for the first contact are: the gauge pressure is 0.07 MPa and the temperature is 91 °C;

[0156] (2) In the second coagulation kettle F2, make the first colloidal particle water have the second contact with the steam II, and separate the material after the second contact to obtain water II and the second colloidal particle water; among them:

[0157] The conditions for the second contact are: the gauge pressure is 0.04 MPa and the temperature is 102 °C;

[0158] Send the second colloidal particle water to the first thickener T1 through the second inter-kettle pump P2 for thickening treatment to obtain water III and the third colloidal particle water, and send the third colloidal particle water to the third coagulation kettle F3;

[0159] Send the first part of the water III (fixed flow rate of 18 m 3 / h) as the recycled water to the first coagulation kettle F1 in step (1) for the first contact, and the amount of the recycled water is 15% by volume of the total water volume;

[0160] (3) In the third coagulation kettle F3, the third colloidal particle water is brought into third contact with steam III, and the material after the third contact is separated to obtain water IV and fourth colloidal particle water; the fourth colloidal particle water is sent to the post-treatment unit 4 via the third kettle-to-kettle pump P3; wherein:

[0161] The conditions for the third contact are: gauge pressure is 0.01 MPa and temperature is 100 °C;

[0162] Steam I and steam II are provided by steam 3; steam III is provided by backwashing steam 7; the first concentrator T1 is backwashed by the backwashing steam 7 and backwashing hot water 8;

[0163] The gas phase separated in step (3) (the gas phase at the top of the third coagulation kettle F3) is returned to the middle of the second coagulation kettle F2 via the first steam ejector W1 along with the steam for the air extractor 6 for the second contact;

[0164] The gas phase separated in step (2) (the gas phase at the top of the second coagulation kettle F2) is returned to the middle of the first coagulation kettle F1 via the second steam ejector W2 along with the steam for the air extractor 5 for the first contact;

[0165] The second part of the water III in step (2) is circulated to step (1) as a cleaning liquid to clean the hydraulic pressure filter 9, and the cleaning liquid after cleaning is sent to the first coagulation kettle F1 as coagulation water for the first contact;

[0166] Water I, water II and water IV are circulated to the first coagulation kettle F1 in step (1) as coagulation water for the first contact;

[0167] The gas phase separated in step (1) (the gas phase at the top of the first coagulation kettle F1) successively enters the oil-water separation tank 14 through the cooler 12 and the water cooler 13 for oil-water separation to recover the solvent oil 11 for recycling, and the recovered solvent oil 11 is stored in the oil tank 15.

[0168] After calculation, this device and method save 0.36 t / h of steam, and the steam consumption is reduced by 10%; after concentration, the colloidal particle density is increased by 17.5%, the residence time of the colloidal particles in the third coagulation kettle is increased by 0.17 h, and the oil content in the fourth colloidal particle water is decreased by 0.03%. After operating for 1 month, the number of filter cleanings of this device is 30, and the volume of each filter is 0.15 m 3 , wherein, the solvent oil content in the hydraulic pressure filter is 85% by weight. By using the method of replacing the solvent oil with the hydraulic pressure filter, the solvent oil consumption is reduced by 2 t per month. Calculated at 7700 yuan / t for hexane, the cost is saved by 15,000 yuan. While reducing the solvent consumption, it can also reduce the emission of VOCs during the process of replacing the filter.

[0169] Example 2

[0170] The rubber polymer is coagulated according to the device and method of Example 1, with the difference that:

[0171] In step (1), the rubber polymer solution is a rare earth cis-polybutadiene rubber solution;

[0172] In step (2), the first part of water III (fixed flow rate of 25 m 3 / h) is recycled to the first coagulation kettle F1 in step (1) as recycled water through the first booster pump P4 for the first contact. The amount of this recycled water is 21% by volume of the total water volume;

[0173] The rest are the same. After calculation, this device and method save 0.45 t / h of steam; after concentration, the density of the rubber particles increases by 24.2%, the residence time of the rubber particles in the third coagulation kettle increases by 0.24 h, and the oil content in the fourth rubber particle water decreases by 0.04%. After operating for 1 month, the number of filter cleanings for this device is 15, and the volume of each filter is 0.12 m 3 , among which, the solvent oil content in the oil pressure filter is 90%. By using a water pressure filter to replace the solvent oil, the solvent oil consumption is reduced by 1.34 t per month. Calculated at 7700 yuan / t for hexane, the cost is saved by 0.8 ten thousand yuan. While reducing the solvent consumption, it can also reduce the emission of VOC during the filter replacement process.

[0174] Example 3

[0175] The rubber polymer is coagulated by using the device as Figure 2 shown, and the specific method is as follows:

[0176] (1) The rubber polymer solution from the rubber tank 10 is filtered by the water pressure filter 9, and then in the first coagulation kettle F1, the filtered rubber liquid 2 is brought into the first contact with the coagulation water and steam I, and the material after the first contact is separated to obtain water I and the first rubber particle water;

[0177] Among them, the rubber polymer solution is a nickel-based cis-polybutadiene rubber solution (the content of the rubber polymer is 15% by weight), and the coagulation water includes the sprayed hot water 1 from the post-treatment unit 4;

[0178] The conditions for the first contact are: gauge pressure of 0.075 MPa and temperature of 92 °C;

[0179] The first rubber particle water is sent to the second concentrator T2 through the first inter-kettle pump P1 for concentration treatment to obtain concentrated water and concentrated rubber particle water. The concentrated water (flow rate of 15 m 3 / h) is sent to the post-treatment unit 4; the concentrated rubber particle water is sent to the second coagulation kettle F2;

[0180] (2) In the second coagulation kettle F2, the concentrated colloidal particle water is brought into second contact with steam II, and the material after the second contact is separated to obtain water II and second colloidal particle water; wherein:

[0181] The conditions for the second contact are: gauge pressure is 0.05 MPa and temperature is 102 °C;

[0182] The second colloidal particle water is sent to the first concentrator T1 through the second inter-kettle pump P2 for concentration treatment to obtain water III and third colloidal particle water, and the third colloidal particle water is sent to the third coagulation kettle F3;

[0183] Through the first booster pump P4, the first part of water III (fixed flow rate 18 m 3 / h) is recycled as recycled water to the first coagulation kettle F1 in step (1) for the first contact, and the amount of this recycled water is 15 vol% of the total water volume;

[0184] (3) In the third coagulation kettle F3, the third colloidal particle water is brought into third contact with steam III, and the material after the third contact is separated to obtain water IV and fourth colloidal particle water; wherein:

[0185] The conditions for the third contact are: gauge pressure is 0.01 MPa and temperature is 99 °C;

[0186] The fourth colloidal particle water is sent to the third concentrator T3 through the third inter-kettle pump P3 for concentration treatment to obtain water V and fifth colloidal particle water;

[0187] Through the second booster pump P6, the first part of water V (fixed flow rate 15 m 3 / h) is recycled as recycled water to step (2) for the second contact, and the amount of this recycled water is 12.5 vol% of the total water volume; the fifth colloidal particle water is sent to the post-treatment unit 4; the second part of water V is recycled to step (1) for the first contact;

[0188] Steam I and steam II are provided by steam 3; steam III is provided by backwashing steam 7; the first concentrator T1 is backwashed by backwashing steam 7 and backwashing hot water 8;

[0189] The gas phase separated in step (3) (the gas phase at the top of the third coagulation kettle F3) is returned to the middle of the second coagulation kettle F2 through the first steam ejector W1 along with the air ejector steam 6 for the second contact;

[0190] The gas phase separated in step (2) (the gas phase at the top of the second coagulation kettle F2) is returned to the middle of the first coagulation kettle F1 through the second steam ejector W2 along with the air ejector steam 5 for the first contact;

[0191] The second part of the water III in step (2) is circulated as a cleaning liquid to step (1) to clean the hydraulic pressure filter 9, and the cleaning liquid after cleaning is sent to the first coagulation kettle F1 as condensed water for the first contact;

[0192] Water I, water II, and water IV are circulated as coagulation water to the first coagulation kettle F1 in step (1) for the first contact;

[0193] The gas phase separated in step (1) (the gas phase at the top of the first coagulation kettle F1) enters the oil-water separation tank 14 through the cooler 12 and the water cooler 13 in sequence for oil-water separation to recover the solvent oil 11 for recycling, and the recovered solvent oil 11 is stored in the oil tank 15.

[0194] After calculation, the device and method save 0.56 t / h of steam; after concentration, the density of the rubber particles increases by 17.5%, the residence time of the rubber particles in the third coagulation kettle increases by 0.17 h, and the oil content in the fifth rubber particle water decreases by 0.03%. The device and method can further reduce the consumption of coagulation steam.

[0195] Example 4

[0196] Using the device as shown in Figure 3 to carry out the coagulation of rubber polymers, the specific method is as follows:

[0197] (1) The rubber polymer solution from the rubber tank 10 is filtered by the hydraulic pressure filter 9, and then in the first coagulation kettle F1, the filtered rubber solution 2 is brought into the first contact with the coagulation water and steam I, and the material after the first contact is separated to obtain water I and the first rubber particle water;

[0198] Among them, the rubber polymer solution is a nickel-based cis-butadiene rubber solution (the content of the rubber polymer is 15% by weight), and the coagulation water includes the spray hot water 1 from the post-treatment unit 4;

[0199] The conditions for the first contact are: gauge pressure is 0.06 MPa, and the temperature is 92 °C;

[0200] The first rubber particle water is sent to the second concentrator T2 through the first inter-kettle pump P1 for concentration treatment to obtain concentrated water and concentrated rubber particle water. The concentrated water (flow rate 15 m 3 / h) is sent to the post-treatment unit 4; the concentrated rubber particle water is sent to the second coagulation kettle F2;

[0201] (2) In the second coagulation kettle F2, the concentrated rubber particle water is brought into the second contact with steam II, and the material after the second contact is separated to obtain water II and the second rubber particle water; among them:

[0202] The conditions for the second contact are: gauge pressure is 0.04 MPa, and the temperature is 102 °C;

[0203] The second colloidal particle water is sent to the first concentrator T1 through the second between-kettle pump P2 for concentration treatment to obtain water III and the third colloidal particle water, and the third colloidal particle water is sent to the third coagulation kettle F3;

[0204] Through the first booster pump P4, the first part of water III (fixed flow rate of 18 m 3 / h) is recycled as recycled water to the first coagulation kettle F1 in step (1) for the first contact, and the amount of this recycled water is 15 vol% of the total water volume;

[0205] (3) In the third coagulation kettle F3, the third colloidal particle water is brought into the third contact with steam III, and the material after the third contact is separated to obtain water IV and the fourth colloidal particle water; the fourth colloidal particle water is sent to the fourth coagulation kettle F4 through the third between-kettle pump P3; where:

[0206] The conditions for the third contact are: gauge pressure of 0.02 MPa and temperature of 100 °C;

[0207] (4) In the fourth coagulation kettle F4, the fourth colloidal particle water is brought into the fourth contact with steam IV, and the material after the fourth contact is separated to obtain water VI and the sixth colloidal particle water; where:

[0208] The conditions for the fourth contact are: gauge pressure of 0.01 MPa and temperature of 99 °C;

[0209] The sixth colloidal particle water is sent to the third concentrator T3 through the fourth between-kettle pump P7 for concentration treatment to obtain water VII and the seventh colloidal particle water;

[0210] Through the second booster pump P6, the first part of water VII (fixed flow rate of 15 m 3 / h) is recycled as recycled water to step (2) for the second contact, and the amount of this recycled water is 12.5 vol% of the total water volume; the seventh colloidal particle water is sent to the post-treatment unit 4; the second part of water VI and water VII is recycled to step (1) for the first contact;

[0211] Steam I and steam II are provided by steam 3; steam III and steam IV are provided by backwashing steam 7; the first concentrator T1 is backwashed by backwashing steam 7 and backwashing hot water 8;

[0212] The gas phase separated in step (4) (the gas phase at the top of the fourth coagulation kettle F4) and the gas phase separated in step (3) (the gas phase at the top of the third coagulation kettle F3) are returned to the middle of the second coagulation kettle F2 through the first steam ejector W1 along with the gas ejector steam 6 for the second contact;

[0213] Return the gas phase separated in step (2) (the gas phase at the top of the second coagulation kettle F2) to the middle part of the first coagulation kettle F1 through the second steam ejector W2 with the steam 5 of the air ejector for the first contact;

[0214] Return the second part of the water III in step (2) to step (1) as the cleaning liquid to clean the hydraulic pressure filter 9, and send the cleaned cleaning liquid to the first coagulation kettle F1 as the coagulation water for the first contact;

[0215] Return water I, water II and water IV to the first coagulation kettle F1 in step (1) as the coagulation water for the first contact;

[0216] The gas phase separated in step (1) (the gas phase at the top of the first coagulation kettle F1) enters the oil-water separation tank 14 through the cooler 12 and the water cooler 13 in sequence for oil-water separation to recycle the solvent oil 11, and the recycled solvent oil 11 is stored in the oil tank 15.

[0217] After calculation, the device and method save 0.56 t / h of steam; after concentration, the density of the rubber particles increases by 17.5%, the residence time of the rubber particles in the third and fourth coagulation kettles increases by 0.67 h, and the oil content in the seventh rubber particle water decreases by 0.08%. The device and method can further reduce the consumption of the coagulation solvent.

[0218] It can be seen from the above results that by using the device and method provided by the present invention, the energy-saving effect of reducing steam consumption and the consumption reduction effect of reducing solvent consumption can be achieved, the cost is lower, the backwater consumption is stable, the operation cycle is long, and the device utilization rate can also be improved. In addition, the device and method provided by the present invention can also reduce the emissions of light hydrocarbons in coagulation and post-treatment, improve the environment around the device, and reduce carbon emissions.

[0219] The preferred embodiments of the present invention have been described in detail above. However, the present invention is not limited thereto. Within the scope of the technical concept of the present invention, various simple modifications can be made to the technical solutions of the present invention, including any other suitable combination of each technical feature. These simple modifications and combinations should also be regarded as the content disclosed by the present invention and fall within the protection scope of the present invention.

Claims

1. A method for rubber polymer coagulation, characterized in that, The method includes: (1) Filtering the rubber polymer solution with a hydraulic pressure filter, then making a first contact between the filtered glue liquid, condensed water, and steam I, and separating the material after the first contact to obtain water I and first colloidal particle water; (2) Making a second contact between the first colloidal particle water and steam II, and separating the material after the second contact to obtain water II and second colloidal particle water; Concentrating the second colloidal particle water to obtain water III and third colloidal particle water; (3) Making a third contact between the third colloidal particle water and steam III, and separating the material after the third contact to obtain water IV and fourth colloidal particle water; Wherein, a first part of the water III in step (2) is recycled as recycled water to step (1) through a first booster pump for the first contact; the amount of the recycled water is 15 - 40% by volume of the total water volume.

2. The method according to claim 1, wherein, In step (1), the conditions for the first contact include: gauge pressure of 0.06 - 0.08 MPa and temperature of 85 - 95 °C; in step (2), the conditions for the second contact include: gauge pressure of 0.03 - 0.05 MPa and temperature of 100 - 105 °C; in step (3), the conditions for the third contact include: gauge pressure of 0 - 0.02 MPa and temperature of 95 - 100 °C; Preferably, the rubber polymer solution is at least one of nickel-based cis-butadiene rubber solution, rare earth cis-butadiene rubber solution, rare earth isoprene rubber solution, and styrene-butadiene rubber solution; the solvent in the rubber polymer solution is hexane and / or cyclohexane; in the rubber polymer solution, the content of the rubber polymer is 15 - 20% by weight; Preferably, a second part of the water III in step (2) is recycled as a cleaning liquid to step (1) to clean the hydraulic pressure filter, and the cleaning liquid after cleaning is used as condensed water for the first contact; Preferably, at least one of the water I, the water II, and the water IV is recycled as condensed water to step (1) for the first contact.

3. The method according to claim 1 or 2, wherein Return the gas phase separated in step (3) to step (2) for the second contact; return the gas phase separated in step (2) to step (1) for the first contact; Preferably, step (1) further includes: concentrating the first colloidal particle water to obtain concentrated water and concentrated colloidal particle water, and in step (2), making the second contact between the concentrated colloidal particle water and the steam II.

4. The method according to any one of claims 1 to 3, wherein The method further includes: concentrating the fourth colloidal particle water in step (3) to obtain water V and fifth colloidal particle water; Preferably, the method further includes: recycling a first part of the water V as recycled water to step (2) through a second booster pump for the second contact; the amount of the recycled water is 10 - 20% by volume of the total water volume; Preferably, recycle a second part of the water V to step (1) for the first contact.

5. The method according to any one of claims 1-3, wherein, The method further includes: subjecting the fourth colloidal particle water in step (3) to a fourth contact with steam IV, and separating the material after the fourth contact to obtain water VI and sixth colloidal particle water; Preferably, the method further includes: concentrating the sixth colloidal particle water to obtain water VII and seventh colloidal particle water; circulating a first portion of the water VII as recycled water to step (2) through a second booster pump for the second contact; the amount of the recycled water being 10-20% by volume of the total water volume; Preferably, the conditions for the fourth contact include: gauge pressure of 0-0.02 MPa and temperature of 95-100 °C; Preferably, the separated gas phase is returned to step (2) for the second contact; Preferably, a second portion of the water VI and / or the water VII is recycled to step (1) for the first contact.

6. An apparatus for rubber polymer coagulation, characterized in that, The device includes a hydraulic pressure filter, a first coagulation kettle, a second coagulation kettle, and a third coagulation kettle connected in series in sequence; wherein: A first concentrator is provided between the second coagulation kettle and the third coagulation kettle. The inlet of the first concentrator is connected to the colloidal particle water outlet of the second coagulation kettle, the concentrated colloidal particle water outlet of the first concentrator is connected to the inlet of the third coagulation kettle, and the concentrated water outlet of the first concentrator is connected to the inlet of the first coagulation kettle; a first booster pump is further provided between the first concentrator and the first coagulation kettle.

7. The apparatus according to claim 6, wherein, The steam outlet of the third coagulation kettle is connected to the inlet of the second coagulation kettle; a first steam ejector is further provided between the steam outlet of the third coagulation kettle and the inlet of the second coagulation kettle; Preferably, the steam outlet of the second coagulation kettle is connected to the inlet of the first coagulation kettle; a second steam ejector is further provided between the steam outlet of the second coagulation kettle and the inlet of the first coagulation kettle.

8. The device according to claim 6 or 7, wherein, The concentrated water outlet of the first concentrator is connected to the cleaning inlet of the hydraulic pressure filter; the cleaning outlet of the hydraulic pressure filter is connected to the inlet of the first coagulation kettle; Preferably, a cooler, a water cooler, and an oil-water separation tank are sequentially provided at the steam outlet of the first coagulation kettle; Preferably, a second concentrator is further provided between the first coagulation kettle and the second coagulation kettle. The inlet of the second concentrator is connected to the colloidal particle water outlet of the first coagulation kettle, and the concentrated colloidal particle water outlet of the second concentrator is connected to the inlet of the second coagulation kettle.

9. The device according to any one of claims 6 - 8, wherein, A third concentrator is further provided at the colloidal particle water outlet of the third coagulation kettle. The inlet of the third concentrator is connected to the colloidal particle water outlet of the third coagulation kettle, and the concentrated water outlet of the third concentrator is connected to the inlet of the second coagulation kettle; Preferably, a second booster pump is further provided between the third concentrator and the second coagulation kettle.

10. The apparatus according to any one of claims 6 - 8, wherein, The device further includes a fourth coagulation kettle, and the inlet of the fourth coagulation kettle is connected to the colloidal particle water outlet of the third coagulation kettle; Preferably, a third concentrator is further provided at the colloidal particle water outlet of the fourth coagulation kettle. The inlet of the third concentrator is connected to the colloidal particle water outlet of the fourth coagulation kettle, and the concentrated water outlet of the third concentrator is connected to the inlet of the second coagulation kettle; Preferably, a second booster pump is further provided between the third concentrator and the second coagulation kettle; Preferably, the steam outlet of the fourth coagulation kettle is communicated with the inlet of the first steam ejector.

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