CN116747785A - Cooling and purifying device and cooling and purifying system for isocyanate carbonylation intermediate - Google Patents
Cooling and purifying device and cooling and purifying system for isocyanate carbonylation intermediate Download PDFInfo
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- CN116747785A CN116747785A CN202310883412.3A CN202310883412A CN116747785A CN 116747785 A CN116747785 A CN 116747785A CN 202310883412 A CN202310883412 A CN 202310883412A CN 116747785 A CN116747785 A CN 116747785A
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- 238000001816 cooling Methods 0.000 title claims abstract description 108
- 238000005810 carbonylation reaction Methods 0.000 title claims abstract description 43
- 230000006315 carbonylation Effects 0.000 title claims abstract description 41
- 239000012948 isocyanate Substances 0.000 title claims abstract description 12
- 150000002513 isocyanates Chemical class 0.000 title claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 90
- 239000002245 particle Substances 0.000 claims abstract description 73
- 238000005406 washing Methods 0.000 claims abstract description 73
- 239000000463 material Substances 0.000 claims abstract description 58
- 239000007921 spray Substances 0.000 claims abstract description 52
- 238000003756 stirring Methods 0.000 claims abstract description 47
- 238000009423 ventilation Methods 0.000 claims abstract description 36
- 239000007791 liquid phase Substances 0.000 claims abstract description 30
- 238000005469 granulation Methods 0.000 claims abstract description 27
- 230000003179 granulation Effects 0.000 claims abstract description 27
- 238000000746 purification Methods 0.000 claims abstract description 24
- 239000007789 gas Substances 0.000 claims description 47
- 230000008018 melting Effects 0.000 claims description 44
- 238000002844 melting Methods 0.000 claims description 44
- 239000011261 inert gas Substances 0.000 claims description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 30
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 24
- 238000002347 injection Methods 0.000 claims description 13
- 239000007924 injection Substances 0.000 claims description 13
- 238000002386 leaching Methods 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 12
- 239000007787 solid Substances 0.000 claims description 9
- 238000005507 spraying Methods 0.000 claims description 9
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 6
- JYYOBHFYCIDXHH-UHFFFAOYSA-N carbonic acid;hydrate Chemical compound O.OC(O)=O JYYOBHFYCIDXHH-UHFFFAOYSA-N 0.000 claims description 6
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 239000012071 phase Substances 0.000 claims description 5
- 238000010926 purge Methods 0.000 claims description 5
- 239000000243 solution Substances 0.000 claims description 5
- 239000013014 purified material Substances 0.000 claims description 4
- 230000003746 surface roughness Effects 0.000 claims description 4
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 3
- 239000001569 carbon dioxide Substances 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 21
- 239000013078 crystal Substances 0.000 abstract description 14
- 238000009826 distribution Methods 0.000 abstract description 10
- 238000005054 agglomeration Methods 0.000 abstract description 7
- 230000002776 aggregation Effects 0.000 abstract description 7
- 230000003321 amplification Effects 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 238000003199 nucleic acid amplification method Methods 0.000 abstract description 6
- 239000000725 suspension Substances 0.000 abstract description 6
- 238000002425 crystallisation Methods 0.000 abstract description 5
- 230000008025 crystallization Effects 0.000 abstract description 5
- 230000009286 beneficial effect Effects 0.000 abstract description 4
- 239000000543 intermediate Substances 0.000 description 54
- 230000000694 effects Effects 0.000 description 12
- 230000003044 adaptive effect Effects 0.000 description 8
- 239000012535 impurity Substances 0.000 description 7
- 238000000197 pyrolysis Methods 0.000 description 5
- 230000005484 gravity Effects 0.000 description 4
- 239000012768 molten material Substances 0.000 description 4
- 238000004062 sedimentation Methods 0.000 description 4
- 239000011343 solid material Substances 0.000 description 4
- 239000002699 waste material Substances 0.000 description 4
- YGYAWVDWMABLBF-UHFFFAOYSA-N Phosgene Chemical compound ClC(Cl)=O YGYAWVDWMABLBF-UHFFFAOYSA-N 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 239000000155 melt Substances 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- RFGIRNPIHVIBKJ-UHFFFAOYSA-N 6-aminohexyl carbamate Chemical compound NCCCCCCOC(N)=O RFGIRNPIHVIBKJ-UHFFFAOYSA-N 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 2
- 238000000889 atomisation Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000010008 shearing Methods 0.000 description 2
- 238000004065 wastewater treatment Methods 0.000 description 2
- VWKWKTYIJCBWHW-UHFFFAOYSA-N N=C=O.ClC(Cl)=O Chemical compound N=C=O.ClC(Cl)=O VWKWKTYIJCBWHW-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 230000005587 bubbling Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000007806 chemical reaction intermediate Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000003480 eluent Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
- B01J2/02—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops
- B01J2/04—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops in a gaseous medium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
- B01J2/02—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops
- B01J2/06—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops in a liquid medium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/10—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/10—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
- B08B3/102—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration with means for agitating the liquid
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The invention provides a cooling and purifying device and a cooling and purifying system for an isocyanate carbonylation intermediate, wherein the cooling and purifying device comprises a cylinder, the bottom of the cylinder is of a conical structure, a liquid outlet is arranged at the position, close to the tip, of the conical structure, and the cylinder is internally divided into a spray granulation area and a liquid phase washing area in sequence along the trend of materials; the spray granulation zone comprises a granulation system and a cooling system which are sequentially arranged along the trend of the material; the liquid phase washing area comprises a stirring system and an air ventilation piece which are sequentially arranged along the trend of the materials, and the air ventilation piece is arranged in the conical structure and is close to the liquid outlet. The invention realizes stable control and purification of the continuous cooling particle size of the carbonylation molten intermediate by adopting a method combining spray granulation, spray cooling and suspension particle liquid phase washing through the specific design of the spray granulation area and the liquid phase washing area, solves the problems of agglomeration and wider crystal size distribution in the rapid cooling crystallization process, is beneficial to continuous high-efficiency production and is easy for engineering amplification.
Description
Technical Field
The invention belongs to the technical field of fine chemical purification, relates to a cooling and purifying device and a cooling and purifying system for an isocyanate carbonylation intermediate, and particularly relates to a continuous cooling and purifying device and system for a special isocyanate carbonylation intermediate by a non-phosgene method.
Background
The special isocyanate technology by non-phosgene method is to obtain special isocyanate mainly by carbonylation and pyrolysis without using highly toxic phosgene as raw material, and has the characteristics of low cost and high safety.
The non-phosgene isocyanate carbonylation intermediate is generally obtained by multistage rectification and water washing of carbonylation reaction feed liquid. In the water washing purification part, molten carbonylation liquid is usually directly led into water liquid and can be divided into two modes of cold washing and hot washing, wherein the cold washing is the rapid cooling washing of the molten carbonylation liquid in the water liquid, and the problems of agglomeration of reaction intermediates, uneven crystal size, insufficient contact with the water liquid, poor water washing effect, more water consumption, multiple circulation of the water liquid and the like usually occur in the washing process; the heat washing is to keep the carbonylation liquid in a molten state in water for continuous washing, water is usually separated by adopting an oil-water separation mode after the heat washing, and the carbonylation intermediate in the carbonylation liquid has high solubility in the hot water, so that the problem of low yield of the carbonylation intermediate in the purification process can be caused, and the large-scale amplification and continuous production of the cooling and purifying device are seriously influenced by the two washing modes.
Therefore, there is a need to design and develop a cooling and purifying device and a cooling and purifying system for an isocyanate carbonylation intermediate, which overcome the defects of the prior art so as to meet the practical application requirements.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide a cooling and purifying device and a cooling and purifying system for an isocyanate carbonylation intermediate.
To achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the invention provides a cooling and purifying device for an isocyanate carbonylation intermediate, which comprises a barrel, wherein the bottom of the barrel is of a conical structure, a liquid outlet is arranged at a position, close to a tip, of the conical structure, and the interior of the barrel is sequentially divided into a spray granulation area and a liquid phase washing area along the trend of materials; the spray granulation zone comprises a granulation system and a cooling system which are sequentially arranged along the trend of the material, and an exhaust port is arranged on the side wall of the cylinder between the granulation system and the cooling system; the liquid phase washing zone comprises a stirring system and an air ventilation piece which are sequentially arranged along the trend of the material, an overflow port is arranged on the side wall of the barrel between the stirring system and the air ventilation piece, and the air ventilation piece is arranged in the conical structure and is close to the liquid outlet.
In the invention, by specifically designing a spray granulation area and a liquid phase washing area, stable control and purification of the particle size of continuous cooling particles of the carbonylation molten intermediate are realized by adopting a method combining spray granulation, spray cooling and suspension particle liquid phase washing, the problems of agglomeration and wider crystal size distribution in the rapid cooling crystallization process are solved, and the continuous high-efficiency production is facilitated, and the engineering amplification is easy.
The material and the size of the cylinder are not particularly limited, and can be adaptively adjusted according to actual conditions by a person skilled in the art.
It should be noted that, the specific sizes, shapes and numbers of the feed inlet, the air inlet, the liquid outlet, the air outlet and the overflow outlet are not limited in the invention, and those skilled in the art can make adaptive adjustment according to practical situations, and the design similar to the invention falls within the protection scope of the invention.
As a preferable technical scheme of the invention, the top of the cylinder body is respectively provided with a feed inlet and an air inlet.
In the invention, the feeding port and the air inlet are arranged at the top of the cylinder body and can be matched with the components in the cylinder body, so that better spraying force of materials and gas phase is achieved.
Preferably, the granulating system comprises an ejector, a baffling cylinder and a guide cylinder, wherein the ejector is arranged close to the feeding hole, the baffling cylinder is arranged above the guide cylinder, and one end, away from the baffling cylinder, of the guide cylinder is arranged in a liquid phase in the liquid phase washing zone.
The invention ensures the effects of injection of molten material liquid, high-shear particle forming of inert gas, rapid cooling by spraying of a spray cooler and atomization washing by the specific structural design of the injector, the baffle cylinder and the guide cylinder, and achieves the aims of uniform particle forming of the molten material liquid and sufficient contact cooling of washing liquid and particles.
Preferably, the ejector is an ejector sleeve, the ejector sleeve comprises an inner pipe and an outer pipe which are sleeved in sequence from inside to outside, the inner pipe is used for passing materials, and the outer pipe is used for passing gas phase.
It should be noted that, in the present invention, specific materials and numbers of the injection sleeves are not limited, and those skilled in the art may make adaptive adjustments according to actual situations.
Preferably, the baffle cylinder is an annular baffle cylinder.
Preferably, the annular edge of the annular baffle cylinder is fixedly connected with the inner surface of the cylinder body.
Preferably, the annular baffle cylinder and the injector are coaxially arranged.
The specific materials and the number of the annular baffle cylinders and the specific arrangement of the baffle plates are not particularly limited, and can be adaptively adjusted according to practical situations by a person skilled in the art.
Preferably, the guide cylinder comprises an upper guide cylinder and a lower guide cylinder which are sequentially arranged along the trend of the material.
Preferably, the upper guide sleeve comprises a large diameter end and a small diameter end.
Preferably, the edge of the large diameter end is fixedly connected with the inner surface of the cylinder, the small diameter end is fixedly connected with the lower guide cylinder, and one end of the lower guide cylinder, which is far away from the upper guide cylinder, is arranged in the liquid phase washing zone.
The edge of the large-diameter end of the guide cylinder is fixedly connected with the inner surface of the cylinder, the small-diameter end of the guide cylinder is fixedly connected with the guide cylinder, the guide cylinder is in an inverted circular truncated cone shape, and the guide effect of liquid phase is improved by matching with the specific design of the guide cylinder.
It should be noted that, the specific materials and the number of the guide barrels are not particularly limited in the invention, and those skilled in the art can make adaptive adjustment according to actual situations.
Preferably, the exhaust port is disposed at one side of the cylinder corresponding to the upper guide cylinder.
Preferably, the overflow port is disposed at one side of the cylinder corresponding to the guide flow cylinder.
In the invention, the top feeding and side overflow discharging modes are adopted, so that the overall trend of the material is stable, and the generated crystals or particles are completely purified, so that the problems of caking and wider crystal size distribution are avoided.
In a preferred embodiment of the present invention, the injector is provided with at least one, for example, 1, 2, 3, 4, 5, etc., but not limited to the recited values, and other non-recited values within the range are equally applicable.
Preferably, an end of the injector, which is far away from the feed inlet, is provided with an injection hole.
Preferably, the top of the baffle cylinder is disposed above the injection hole.
Preferably, the diameter of the baffle cylinder is between the diameter of the large diameter end and the diameter of the small diameter end.
The diameter of the baffle cylinder is between the diameter of the large diameter end and the diameter of the small diameter end, so that the inert gas sprayed by the sprayer can be enabled to be returned to the sprayer along the area between the baffle cylinder and the inner wall of the purification device after gas-solid separation, small particles formed by spraying can be effectively limited to be returned upwards, the uniformity of the particle size is improved, and the quantity of the sprayed inert gas can be reduced.
Preferably, the inner surface of the upper guide cylinder is smooth.
The roughness of the inner surface of the upper guide cylinder is preferably not more than 0.2. Mu.m, and may be, for example, 0.2. Mu.m, 0.18. Mu.m, 0.16. Mu.m, 0.14. Mu.m, 0.12. Mu.m, 0.1. Mu.m, etc., but is not limited to the values recited, and other values not recited in the numerical range are equally applicable.
The inner surface of the upper guide cylinder is smooth and has the roughness less than or equal to 0.2 mu m, and the design can ensure that solid particles formed by injection can fall to a cooling and washing area under the action of gravity when falling to the upper guide cylinder, so that excessive solid accumulation of the upper guide cylinder is avoided, and the operation stability of the upper injection granulation area is prevented from being influenced.
Preferably, the lower guide cylinder is a straight cylinder.
The diameter of the lower guide cylinder is preferably 0.5 to 0.7 times the maximum diameter of the cylinder, and may be, for example, 0.5 times, 0.55 times, 0.6 times, 0.65 times, 0.7 times, etc., but is not limited to the recited values, and other values not recited in the range of values are equally applicable.
The diameter of the guide flow lower cylinder is 0.5-0.7 times of the maximum diameter of the cylinder, and the design can ensure the washing time of stirring the material particles and the cooling washing liquid in the guide flow lower cylinder by a flat paddle and ensure the time of stirring and suspending by the lower paddle to be fully mixed and stable.
As a preferable technical scheme of the invention, the cooling system comprises an annular pipeline, a spray cooler and a gas filter, wherein the annular pipeline is sleeved at one end of the guide flow cylinder, which is close to the guide flow upper cylinder, the spray cooler is arranged on the annular pipeline, and the gas filter is arranged below the spray cooler.
The specific materials and the number of the annular pipeline, the spray cooler and the gas filter are not particularly limited, and can be adaptively adjusted according to practical situations by a person skilled in the art.
Preferably, the nozzle of the spray cooler is inclined downwards and towards the axis, and is used for cooling the gas and solid particles flowing through the guide lower cylinder.
Preferably, the gas filter is provided on the guide flow down tube.
The gas filter preferably has a filtration accuracy of 1 to 10. Mu.m, for example, 1 μm, 2 μm, 4 μm, 6 μm, 8 μm, 10 μm, etc., but the present invention is not limited to the above-mentioned values, and other values not shown in the above-mentioned range are applicable.
The filtering precision of the gas filter is 1-10 mu m, and the size range can ensure that cooling material particles carried in the gas can be intercepted by 99.9 percent; if the concentration is not within the range, if the filtration precision is too high, part of particles can be directly carried out through a gas phase port without washing, so that the yield and purity are reduced and the circulating gas pressure retraction equipment is damaged; if the filtering precision is too small, the pressure difference between the inside and the outside of the device can be increased, or gas enters the liquid layer and enters the overflow area in a bubbling mode, so that the vibration of the device and the purity of the device are obviously reduced, and the operation stability is affected.
The gas filter in the invention can be an annular filter or a filter formed by combining a plurality of rectangular filter sheets, and spray liquid entering from a liquid inlet can wash the filter, so that the accuracy of the filter is ensured.
Preferably, a liquid inlet is arranged on one side of the cylinder body, which is level with the annular pipeline, and the liquid inlet is connected with the annular pipeline through a liquid inlet pipe.
As a preferable technical scheme of the invention, the stirring system comprises a double-layer stirring paddle, a supporting column and a stirring motor, wherein one end of the supporting column is fixedly connected with the double-layer stirring paddle, the other end of the supporting column penetrates through the liquid outlet to be externally connected with the stirring motor, and the double-layer stirring paddle is electrically connected with the stirring motor.
The specific materials, sizes and numbers of the double-layer stirring paddles, the supporting columns and the stirring motors are not particularly limited, and can be adaptively adjusted according to practical situations by a person skilled in the art.
Preferably, the double-layer stirring paddle is arranged in the guide lower cylinder.
Preferably, the double-layer stirring paddle comprises a flat paddle and an anchor paddle which are sequentially arranged along the material trend.
Preferably, the anchor paddles are V-shaped anchor paddles.
It should be noted that the double-layer stirring paddle is designed in the invention, and the structure is a flat paddle and a V-shaped anchor paddle because the structure is matched with the concrete design of the guide cylinder and the ventilation cone, so that the sedimentation particles are uniformly suspended by adopting bubbles, the particle materials and the washing liquid can be fully stirred and washed in the guide lower cylinder, the washing effect is enhanced, and the bottom sedimentation particles can be stirred and suspended by the air bubble through the cooperation of the V-shaped anchor paddle and the ventilation cone, the mass transfer of solid and liquid is enhanced, the washing effect of the carbonylation intermediate is improved, the particle size uniformity of the particles of the carbonylation intermediate after washing is ensured, and the process is simple, safe and reliable.
Preferably, the flat paddle and the anchor paddle are coaxially disposed, and the distance between the flat paddle and the anchor paddle is 0.16 to 0.25 times the height of the cylinder, for example, 0.16 times, 0.18 times, 0.2 times, 0.22 times, 0.24 times, 0.25 times, etc., but not limited to the recited values, and other non-recited values within the range of values are equally applicable.
The distance between the flat paddle and the anchor paddle is 0.16-0.25 times of the height of the cylinder body, so that most particles can be fully washed under the stirring of the flat paddle in the size range, and a small amount of oversized particles fully settle to the bottom of the purification device and are stirred by the V-shaped anchor paddle to form homogeneous suspension, so that the synergistic effect of the two paddles is better exerted; if it is not within this range, it will result in insufficient washing of a part of the particles, direct carry-over, and insufficient purity of the washed material.
As a preferable technical scheme of the invention, the ventilation piece is a ventilation cone, and the surface of the ventilation cone is provided with a through hole.
In the present invention, the size, number, shape, etc. of the through holes are not particularly limited, and those skilled in the art can adapt to the actual situation.
Preferably, the tip of the vent cone is disposed corresponding to the tip of the cone structure.
Preferably, the through hole is provided with at least one, for example, 1, 2, 3, 4, 5, etc., but not limited to the recited values, and other non-recited values within the range of values are equally applicable.
The diameter of the through hole is preferably 1 to 3mm, and may be, for example, 1mm, 1.5mm, 2mm, 2.5mm, 3mm, etc., but is not limited to the values recited, and other values not recited in the range are equally applicable.
Preferably, an air hole is arranged on the air outlet pipe, and the air hole is used for ventilating the ventilation cone.
The surface roughness of the tapered structure is preferably not more than 0.4. Mu.m, and may be, for example, 0.4. Mu.m, 0.3. Mu.m, 0.2. Mu.m, 0.1. Mu.m, etc., but is not limited to the values recited, and other values not recited in the range are equally applicable.
The surface roughness of the conical structure is less than or equal to 0.4 mu m, so that a small amount of solid materials falling to the bottom of the cone gradually slide to the conical ventilation cone in the range, and the solid materials are suspended again by the ventilation cone and the ventilation; if the amount of the water is not within the range, solid materials are accumulated at the bottom, and the suspension and washing effects of the bottom materials are affected.
As a preferable technical scheme of the invention, the air inlet is used for feeding inert gas, and the inert gas is carbon dioxide and nitrogen.
Preferably, the feed port is for a crude intermediate feed and the crude intermediate is a melting point feed.
The crude intermediate in the present invention refers to crude alkyl dicarbamate, and the melting point of the raw material may be 100 to 120 ℃.
Preferably, the volume ratio of the inert gas to the crude intermediate is (4-10): 1, and may be, for example, 4:1, 5:1, 6:1, 7:1, 8:1, 9:1, 10:1, etc., but is not limited to the recited values, and other non-recited values within the range of values are equally applicable.
The inert gas may be introduced at a temperature of 25 to 60 ℃, for example, 25 ℃, 30 ℃, 35 ℃, 40 ℃, 45 ℃, 50 ℃, 55 ℃, 60 ℃, or the like, but the inert gas is not limited to the values listed, and other values not listed in the range are applicable.
The air inlet temperature of the inert gas is 25-60 ℃, so that the molten intermediate can be rapidly cooled and molded in the range, and meanwhile, the temperature control during spraying can be realized, and the washing effect is enhanced; if the particle size is not within the range, the washing effect is poor, or the particles cannot be molded, and the stable operation and the size regulation of the particles cannot be ensured.
Preferably, the pressure of the inert gas is greater than the pressure of the cooling purification device.
The pressure difference between the inert gas and the cooling/purifying device is preferably 0.05 to 0.2MPa, and may be, for example, 0.05MPa, 0.08MPa, 0.1MPa, 0.13MPa, 0.15MPa, 0.16MPa, 0.18MPa, 0.2MPa, etc., but is not limited to the values listed, and other values not listed in the range are equally applicable.
The pressure difference between the inert gas and the cooling purification device is 0.05-0.2 MPa, so that the molten liquid drops can be subjected to high-shear dispersion in the range, the particle size can be controlled, and the particle size distribution is uniform; if the particle diameter is not within this range, the feed liquid may be cooled to a lump or the particle diameter may be too small.
Preferably, the mass ratio of the spraying amount of the cooling system to the feeding amount of the crude intermediate is (2-4): 1, for example, 2:1, 2.5:1, 3:1, 3.5:1, 4:1, etc., but not limited to the recited values, and other non-recited values within the range of values are equally applicable.
The mass ratio of the spraying amount of the cooling system to the feeding amount of the crude intermediate is (2-4): 1, because the impurity components in the crude intermediate can be fully removed in the range; if the content is not within the range, the purified solid material of the feed liquid cannot meet the purity requirement.
Preferably, the spray liquid adopted by the cooling system is desalted water or dimethyl carbonate.
In the present invention, desalted water is a term commonly used for industrial project water, and can be considered as water quality similar to laboratory deionized water.
In a second aspect, the present invention provides a cooling and purifying system, the cooling and purifying system includes a cooling and purifying device, a centrifugal device and a melting device connected by pipeline in turn, the cooling and purifying device adopts the cooling and purifying device in the first aspect.
As a preferable technical scheme of the invention, the centrifugal device is a centrifugal machine.
In the invention, the type, shape, etc. of the centrifuge are not particularly limited, and those skilled in the art can adjust adaptively according to practical situations.
Preferably, the centrifuge is a two-stage pusher centrifuge.
Preferably, the melting device is a melting tank.
In the present invention, the type, shape, etc. of the melting tank are not particularly limited, and those skilled in the art can adapt to the actual situation.
In a preferred embodiment of the present invention, the mass ratio of the amount of the leaching solution used in the centrifugal device to the material in the inlet is (0.5 to 1): 1, and may be, for example, 0.5:1, 0.6:1, 0.7:1, 0.8:1, 0.9:1, 1:1, etc., but not limited to the recited values, and other non-recited values within the range of values are equally applicable.
The mass ratio of the leaching solution adopted by the centrifugal device to the material at the feed inlet is (0.5-1): 1, because the purity of the carbonylation intermediate crystal can meet the requirement in the range; if outside this range, the purity of the carbonylated intermediate crystal is lowered.
Preferably, the temperature of the melting device is above the melting point of the purge material.
It should be noted that, the purified material refers to crude alkyl dicarbamate, the melting point of which may be 100-120 ℃, and the melting point is set according to the corresponding specific material, and those skilled in the art can understand that the purified material falls within the protection scope of the present invention.
Preferably, the difference between the temperature of the melting device and the melting point of the purge material is 5 to 10 ℃, for example, 5 ℃, 6 ℃, 7 ℃, 8 ℃, 9 ℃, 10 ℃ and the like, but the present invention is not limited to the above-mentioned values, and other values not mentioned in the above-mentioned value range are equally applicable.
The difference between the temperature of the melting device and the melting point of the purified material is 5-10 ℃, because the material can be fully melted in the range, and the water can be fully removed; if the temperature is not in the range, if the temperature is too low, the materials cannot be pumped and the pipeline is easy to be blocked; if the temperature is too high, the material can deteriorate after long-term residence.
Preferably, the leaching solution adopted by the centrifugal device is desalted water or dimethyl carbonate.
Illustratively, the purification process of the cooling purification system of the present invention comprises:
the crude carbonylation intermediate can be obtained after passing through a cooling purification device, a centrifugal device and a melting device in sequence, and then the high-purity melting intermediate is sent to a downstream pyrolysis unit. The inert gas separated by the cooling and purifying device can be reused after being compressed and separated from gas and liquid, the washing liquid separated by the centrifugal device can be reused as a water supplementing part, the surplus part is sent to the wastewater treatment, and the top evaporation gas of the melting device can be reused as the eluent after being condensed.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, through the specific design of the spray granulation area and the liquid phase washing area, the stable control and purification of the particle size of the continuous cooling particles of the carbonylation molten intermediate are realized by adopting a method combining spray granulation, spray cooling and liquid phase washing of suspended particles, the problems of large consumption of washing liquid, large circulation amount, high impurity content, easy agglomeration of the intermediate and uneven particle size distribution in the cold washing process of the conventional carbonylation intermediate washing and purifying device are solved, the problems of low yield and low equivalent rate of the carbonylation intermediate in the hot washing process are solved, the problems of relatively wide agglomeration and crystal size distribution in the rapid cooling crystallization process are solved, and the process is efficient and safe, thereby being beneficial to continuous and efficient production and easy engineering amplification.
Furthermore, the cooling purification device realizes continuous and efficient production of the carbonylation intermediates, the impurity content (except for the washing liquid) can be reduced to less than or equal to 0.2%, the intermediate crystal particle size distribution is narrow to 150-350 mu m, the impurity content (except for the washing liquid) can be reduced to less than or equal to 0.05% after continuous centrifugal leaching, the pyrolysis feeding standard can be met after melt drying, the purity of the carbonylation intermediates can be more than 99.6%, and the yield of the carbonylation intermediates can be more than 99%.
Drawings
FIG. 1 is a schematic view of a cooling and purifying apparatus according to an embodiment of the present invention;
FIG. 2 is a schematic diagram of a cooling and purifying system according to an embodiment of the present invention;
wherein, 1-ejector; 2-a baffle cylinder; 3-a guide cylinder; 4-spray cooler; 5-a gas filter; 6-flat paddles; 7-V-anchor paddles; 8-double-layer stirring paddles; 9-a conical structure; 10-ventilation cone; 11-a stirring motor; 12-cooling and purifying device; 13-a centrifuge device; 14-a melting device;
a-a feeding port; b-an air inlet; c-a liquid inlet; d-air holes; e-a liquid outlet; f-overflow port; g-exhaust port; h-leaching liquid; i-washing liquid; j-evaporating gas; k-carbonylating the molten intermediate; l-recycling liquid.
Detailed Description
It is to be understood that in the description of the present invention, the terms "center", "longitudinal", "lateral", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", etc. indicate orientations or positional relationships based on the drawings, are merely for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the devices or elements referred to must have a specific orientation, be configured and operated in a specific orientation, and thus are not to be construed as limiting the present invention. Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first", "a second", etc. may explicitly or implicitly include one or more such feature. In the description of the present invention, unless otherwise indicated, the meaning of "a plurality" is two or more.
It should be noted that, in the description of the present invention, unless explicitly specified and limited otherwise, the terms "disposed," "connected," and "connected" are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium, and can be communication between two elements. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art in a specific case.
It will be appreciated by those skilled in the art that the present invention necessarily includes the necessary piping, conventional valves and general pumping equipment for achieving the process integrity, but the foregoing is not a major inventive aspect of the present invention, and that the present invention is not particularly limited thereto as the layout may be added by themselves based on the process flow and the equipment configuration options.
The technical scheme of the invention is further described below by the specific embodiments with reference to the accompanying drawings.
In a specific embodiment, the invention provides a cooling and purifying device 12 of an isocyanate carbonylation intermediate, as shown in fig. 1, the cooling and purifying device 12 comprises a cylinder, the top of the cylinder is respectively provided with a feed inlet a and an air inlet b, the bottom of the cylinder is provided with a conical structure 9, the position, close to the tip, of the conical structure 9 is provided with a liquid outlet e, and the inside of the cylinder is sequentially divided into a spray granulation area and a liquid phase washing area along the material trend; the spray granulation zone comprises a granulation system and a cooling system which are sequentially arranged along the trend of the material, and an exhaust port g is arranged on the side wall of the cylinder body between the granulation system and the cooling system; the liquid phase washing zone comprises a stirring system and an air ventilation piece which are sequentially arranged along the trend of the materials, an overflow port f is arranged on the side wall of the barrel body between the stirring system and the air ventilation piece, and the air ventilation piece is arranged in the conical structure 9 and is close to the liquid discharge port e.
In the invention, by specifically designing a spray granulation area and a liquid phase washing area, stable control and purification of the particle size of continuous cooling particles of the carbonylation molten intermediate k are realized by adopting a method of combining spray granulation, spray cooling and suspension particle liquid phase washing, the problems of agglomeration and wider crystal size distribution in the rapid cooling crystallization process are solved, and the continuous high-efficiency production is facilitated, and the engineering amplification is easy.
The material and the size of the cylinder are not particularly limited, and can be adaptively adjusted according to actual conditions by a person skilled in the art.
It should be noted that, the specific sizes, shapes and numbers of the feed port a, the air inlet b, the liquid outlet e, the air outlet g and the overflow port f are not limited in the present invention, and those skilled in the art can make adaptive adjustment according to practical situations, and all the designs similar to the present invention fall within the protection scope of the present invention.
The granulating system comprises an ejector 1, a baffling cylinder 2 and a guide cylinder 3, wherein the ejector 1 is close to a feed port a, the baffling cylinder 2 is arranged above the guide cylinder 3, and one end, away from the baffling cylinder 2, of the guide cylinder 3 is arranged in a liquid phase in the liquid phase washing zone.
The invention ensures the injection of molten material liquid, the high-shear particle forming of inert gas, the rapid cooling and atomization washing effect of spray cooler 4 and realizes the uniform forming of the particles of the molten material liquid and the aim of fully contacting and cooling washing liquid i with the particles by the specific structural design of the injector 1, the baffle cylinder 2 and the guide cylinder 3.
The ejector 1 is an injection sleeve, the injection sleeve comprises an inner pipe and an outer pipe which are sleeved in sequence from inside to outside, the inner pipe is used for passing materials, and the outer pipe is used for passing gas phase. It should be noted that, in the present invention, specific materials and numbers of the injection sleeves are not limited, and those skilled in the art may make adaptive adjustments according to actual situations.
The baffle cylinder 2 is an annular baffle cylinder 2, the annular edge of the annular baffle cylinder 2 is fixedly connected with the inner surface of the cylinder body, and the annular baffle cylinder 2 and the injector 1 are coaxially arranged. It should be noted that, in the present invention, the specific materials, the number and the specific arrangement of the baffle plates of the annular baffle cylinder 2 are not particularly limited, and those skilled in the art can make adaptive adjustment according to actual situations.
The guide cylinder 3 comprises an upper guide cylinder and a lower guide cylinder which are sequentially arranged along the trend of the material, the upper guide cylinder comprises a large-diameter end and a small-diameter end, the edge of the large-diameter end is fixedly connected with the inner surface of the cylinder body, the small-diameter end is fixedly connected with the lower guide cylinder, and one end, far away from the upper guide cylinder, of the lower guide cylinder is arranged in a liquid phase in the liquid phase washing zone.
In the invention, the edge of the large diameter end of the guide cylinder 3 is fixedly connected with the inner surface of the cylinder, the small diameter end is fixedly connected with the guide cylinder, the guide cylinder is in the shape of an inverted circular truncated cone, and the guide effect of the liquid phase is improved by matching with the specific design of the far guide cylinder. It should be noted that, in the present invention, specific materials and numbers of the guide barrels 3 are not limited, and those skilled in the art may make adaptive adjustments according to actual situations.
The exhaust port g is arranged at one side of the cylinder body corresponding to the upper guide cylinder, and the overflow port f is arranged at one side of the cylinder body corresponding to the lower guide cylinder. In the invention, the top feeding and side overflow discharging modes are adopted, so that the overall trend of the material is stable, and the generated crystals or particles are completely purified, so that the problems of caking and wider crystal size distribution are avoided.
The number of the injectors 1 is at least one, and may be, for example, 1, 2, 3, 4, 5, etc., but is not limited to the listed values, and other values not listed in the range are equally applicable.
The injector 1 is provided with an injection hole at one end far away from the feed port a, the top of the baffle cylinder 2 is arranged above the injection hole, the diameter of the baffle cylinder 2 is between the diameter of the large diameter end and the diameter of the small diameter end, the inner surface of the upper guide cylinder is smooth, the roughness of the inner surface of the upper guide cylinder is less than or equal to 0.2 μm, for example, 0.2 μm, 0.18 μm, 0.16 μm, 0.14 μm, 0.12 μm, 0.1 μm and the like, but the invention is not limited to the listed values, and other non-listed values in the range of the values are equally applicable.
The lower guide cylinder is a straight cylinder, and the diameter of the lower guide cylinder is 0.5 to 0.7 times the maximum diameter of the cylinder, for example, 0.5 times, 0.55 times, 0.6 times, 0.65 times, 0.7 times, etc., but the present invention is not limited to the above-mentioned values, and other values not mentioned in the above-mentioned numerical range are applicable.
The cooling system comprises an annular pipeline, a spray cooler 4 and a gas filter 5, wherein the annular pipeline is sleeved at one end of the lower guide cylinder, which is close to the upper guide cylinder, the spray cooler 4 is arranged on the annular pipeline, and the gas filter 5 is arranged below the spray cooler 4. In the present invention, the specific materials and numbers of the annular pipeline, the spray cooler 4 and the gas filter 5 are not particularly limited, and those skilled in the art can adapt to the actual situation.
The spray nozzle of the spray cooler 4 is inclined downwards and faces the axis for cooling the gas and solid particles flowing through the guide lower cylinder, the gas filter 5 is arranged on the guide lower cylinder, and the filtering precision of the gas filter 5 is 1-10 mu m. The liquid inlet c is arranged on one side of the cylinder body, which is level with the annular pipeline, and is connected with the annular pipeline through a liquid inlet pipe.
The stirring system comprises a double-layer stirring paddle 8, a supporting column and a stirring motor 11, wherein one end of the supporting column is fixedly connected with the double-layer stirring paddle 8, the other end of the supporting column penetrates through the liquid outlet e to be externally connected with the stirring motor 11, and the double-layer stirring paddle 8 is electrically connected with the stirring motor 11. In the present invention, the specific materials, sizes and numbers of the double-layer stirring paddle 8, the supporting column and the stirring motor 11 are not particularly limited, and those skilled in the art can make an adaptive adjustment according to actual situations.
The double-layer stirring paddle 8 is arranged in the guide lower cylinder, and the double-layer stirring paddle 8 comprises a flat paddle 6 and an anchor paddle which are sequentially arranged along the trend of the material, and the anchor paddle is a V-shaped anchor paddle 7.
It should be noted that, the double-layer stirring paddle 8 is designed in the invention, and the flat paddle 6 and the V-shaped anchor paddle 7 are in specific design of the draft tube 3 and the ventilation cone 10, so that the sedimentation particles are uniformly suspended by adopting bubbles, the particle materials and the washing liquid i can be fully stirred and washed in the draft tube, the washing effect is enhanced, and the bottom sedimentation particles can be stirred and suspended by the air bubbles through the cooperation of the V-shaped anchor paddle 7 and the ventilation cone 10, so that the mass transfer of solid and liquid is enhanced, the washing effect of the carbonylation intermediate is improved, the particle size uniformity of the carbonylation intermediate after washing is ensured, the process is simple, and the method is safe and reliable.
The flat paddle 6 and the anchor paddle are coaxially provided, and the distance between the flat paddle 6 and the anchor paddle is 0.16 to 0.25 times the height of the cylinder, and may be, for example, 0.16 times, 0.18 times, 0.2 times, 0.22 times, 0.24 times, 0.25 times, or the like, but the present invention is not limited to the recited values, and other values not recited in the numerical range are equally applicable.
The ventilation piece is a ventilation cone, the tip of the ventilation cone 10 is arranged corresponding to the tip of the conical structure 9, and the surface of the ventilation cone 10 is provided with a through hole. In the present invention, the size, number, shape, etc. of the through holes are not particularly limited, and those skilled in the art can adapt to the actual situation.
The number of the through holes may be at least one, for example, 1, 2, 3, 4, 5, etc., but is not limited to the recited values, and other non-recited values within the range of values are equally applicable. The diameter of the through hole is 1 to 3mm, and may be, for example, 1mm, 1.5mm, 2mm, 2.5mm, 3mm, etc., but is not limited to the values listed, and other values not listed in the numerical range are applicable.
An air hole d is arranged on the air outlet pipe of the liquid outlet e of the ventilation cone 10 and is used for ventilating the ventilation cone 10.
The surface roughness of the tapered structure 9 is not more than 0.4. Mu.m, and may be, for example, 0.4. Mu.m, 0.3. Mu.m, 0.2. Mu.m, 0.1. Mu.m, etc., but is not limited to the values recited, and other values not recited in the range are equally applicable.
The gas inlet b is used for feeding inert gas, the inert gas is carbon dioxide and nitrogen, the feed inlet a is used for feeding crude intermediate, the crude intermediate is fed with melting point, the volume ratio of the inert gas to the crude intermediate is (4-10): 1, for example, 4:1, 5:1, 6:1, 7:1, 8:1, 9:1, 10:1 and the like can be adopted, but the method is not limited to the listed numerical values, and other non-listed numerical values in the numerical range are equally applicable.
The inert gas may be introduced at a temperature of 25 to 60 ℃, for example, 25 ℃, 30 ℃, 35 ℃, 40 ℃, 45 ℃, 50 ℃, 55 ℃, 60 ℃, etc., but the inert gas is not limited to the values listed, and other values not listed in the range are applicable.
The pressure of the inert gas is greater than the pressure of the cooling and purifying device 12, and the pressure difference between the inert gas and the cooling and purifying device 12 is 0.05 to 0.2MPa, and may be, for example, 0.05MPa, 0.08MPa, 0.1MPa, 0.13MPa, 0.15MPa, 0.16MPa, 0.18MPa, 0.2MPa, etc., but is not limited to the values listed, and other values not listed in the range of values are equally applicable.
The mass ratio of the spray amount of the cooling system to the feed amount of the crude intermediate is (2 to 4): 1, and may be, for example, 2:1, 2.5:1, 3:1, 3.5:1, 4:1, etc., but is not limited to the recited values, and other non-recited values within the range of values are equally applicable. The spray liquid adopted by the cooling system is desalted water or dimethyl carbonate.
In another embodiment, the invention provides a cooling and purifying system, which comprises a cooling and purifying device 12, a centrifugal device 13 and a melting device 14 which are connected in a pipeline way, wherein the cooling and purifying device 12 adopts the cooling and purifying device 12.
The centrifugal device 13 is a centrifugal machine, and further, the centrifugal machine is a two-stage pusher plate type centrifugal machine. The leaching liquid h adopted by the centrifugal device 13 is desalted water or dimethyl carbonate. In the invention, the type, shape, etc. of the centrifuge are not particularly limited, and those skilled in the art can adjust adaptively according to practical situations.
The melting device 14 is a melting tank. In the present invention, the type, shape, etc. of the melting tank are not particularly limited, and those skilled in the art can adapt to the actual situation.
The mass ratio of the amount of the eluting solution h to the material fed to the inlet a used in the centrifugal device 13 is (0.5 to 1): 1, and may be, for example, 0.5:1, 0.6:1, 0.7:1, 0.8:1, 0.9:1, 1:1, etc., but not limited to the values listed, and other non-listed values within the range of values are equally applicable.
The temperature of the melting device 14 is above the melting point of the purge material. It should be noted that, the melting point in the present invention is set according to the corresponding specific materials, and those skilled in the art can understand that the situation is within the protection scope of the present invention.
The difference between the temperature of the melting device 14 and the melting point of the purge material is 5 to 10 ℃, and may be, for example, 5 ℃, 6 ℃, 7 ℃, 8 ℃, 9 ℃, 10 ℃, or the like, but is not limited to the values listed, and other values not listed in the range are applicable.
Illustratively, the method of using the cooling and purifying apparatus 12 of the present invention, as shown in FIG. 1, includes:
the melt of the crude carbonylation intermediate enters the inner tube of the ejector 1 at the top of the cooling and purifying device 12 through the feed port a, inert gas enters the outer tube of the ejector 1 through the air inlet b, the melt is rapidly dispersed and cooled into particles under the jet shearing of the inert gas, the particles are entrained by the gas to fall down along the baffle cylinder 2, a small part of the gas circularly rises to the ejector 1 along the upper guide cylinder, a large part of the gas falls down to the lower guide cylinder, the spray cooler 4 is used for spray cooling and fully contacting with the particles for washing, most of the particles fall to the bottom liquid layer, and a small amount of the particles are filtered by the gas filter 5 and then discharged as tail gas through the exhaust port g. Under the condition that the flat paddles 6 stir, the particles and the washing liquid i are fully mixed and washed, under the action of gravity, the liquid containing the particles moves downwards, part of larger particles fall to the bottom of the device, the larger particles float upwards under the action of gas in the anchor paddles and the ventilation cone 10, suspended multiphase flow is formed at the bottom of the device for fully washing, and the washed carbonylation intermediate liquid overflows to downstream equipment through the overflow port f.
The crude carbonylation intermediate passes through a cooling purification device 12, a centrifugal device 13 and a melting device 14 in sequence to obtain a high-purity molten intermediate, and then the high-purity molten intermediate is sent to a downstream pyrolysis unit. The inert gas separated by the cooling and purifying device 12 can be recycled after being compressed and gas-liquid separated, the washing liquid i separated by the centrifugal device 13 can be used as water for partial recycling (can be used as recycling liquid l), the surplus part is sent to the wastewater treatment, and the top evaporation gas j of the melting device 14 can be recycled to the centrifugal device 13 after being condensed for use as leaching liquid h.
Further, the purification process of the cooling purification system in the present invention is shown in fig. 2. Comprising the following steps:
the melt liquid of the crude carbonylation intermediate and inert gas enter a cooling and purifying device 12 according to the feed volume ratio of 4:1-10:1, after spray granulation, particles are sprayed by spraying liquid in the middle of the device, the mass ratio of spraying amount to the feed of the intermediate is 2:1-4:1, tail gas is discharged through a gas outlet g, and then can return to a gas inlet b after compression and gas-liquid separation, overflow slurry is subjected to gravity blanking to a centrifugal machine, the centrifugal machine can be arranged into a two-stage form, namely, a one-stage centrifugal form and a two-stage leaching form, and the mass ratio of leaching liquid h to materials in the centrifugal machine is 0.5:1-1:1. The washing liquid i after centrifugation can be used as a supplementary solvent to enter a carbonylation reaction part, and part of the washing liquid i is used as waste liquid to be sent to a waste liquid treatment unit. Discharging the qualified carbonylation intermediate from the centrifugal machine to a melting tank, wherein the temperature of the melting tank is controlled to be about 5-10 ℃ higher than the melting point of the carbonylation intermediate material.
Example 1
The present embodiment provides a purification method of a cooling purification system, wherein:
1, 6-hexamethylene dicarbamate HDC (containing impurities of aminohexyl carbamate HMC and N-methylated aminohexyl carbamate N-HMC 8%) enters an inner tube of the ejector 1 through a feed port a, nitrogen enters an outer tube of the ejector 1 through a gas inlet b, HDC liquid and nitrogen are fed according to a feed volume ratio of 5:1, under the jet shearing of the nitrogen, the molten liquid is rapidly dispersed and cooled into particles, the primary particle size of the particles is 200 mu m, the nitrogen is entrained with the particles to fall down along a baffle cylinder 2, a small part of the nitrogen is circularly lifted to the ejector 1 along a guide upper cylinder, a large part of the nitrogen falls down to a guide lower cylinder, and is sprayed and cooled by a spray cooler 4, so that the water liquid and the particles are fully contacted and washed, the mass ratio of the spray water liquid to the feed of an intermediate is 2.5:1, most of the particles fall to a bottom liquid layer, a small amount of the particles entrained by the nitrogen are filtered by a gas filter 5, and the residual nitrogen is discharged as tail gas through a gas outlet g.
Under the condition that the flat paddles 6 stir, the particles and the washing liquid i are fully mixed and washed, under the action of gravity, the liquid containing the particles moves downwards, part of larger particles fall to the bottom of the device at about 350 mu m, under the action of nitrogen in the anchor paddles and the ventilation cone 10, the larger particles float upwards, suspended multiphase flow is formed at the bottom of the device for fully washing, and the washed carbonylation intermediate liquid overflows to the centrifugal machine through the overflow port f.
The particle size is basically controlled at 260 mu m, the centrifugal machine is a two-stage push plate type centrifugal machine, and the mass ratio of water to liquid in the centrifugal machine is 0.5:1. The centrifuged washing water is sent to a waste liquid treatment unit as waste liquid. The aqueous solids enter a melting tank at a melting temperature of 120 ℃ and are fed to a downstream pyrolysis unit after melting.
The grain size range of the crystals treated by the purification cooling system is 200-300 mu m, the impurity content of HMC and N-HMC in the 1, 6-hexamethylene dicarbamate is reduced to 0.15%, the impurity content is further reduced to 0.04% after centrifugal leaching, and the yield of the 1, 6-hexamethylene dicarbamate in the cooling purification process is 99.1%.
In summary, the invention realizes stable control and purification of the particle size of the continuous cooling particles of the carbonylation molten intermediate k by adopting a method combining spray granulation, spray cooling and suspension particle liquid phase washing through the specific design of the spray granulation area and the liquid phase washing area, solves the problems of agglomeration and wider crystal size distribution in the rapid cooling crystallization process, is beneficial to continuous high-efficiency production and is easy for engineering amplification.
The foregoing is merely illustrative of the present invention, and the present invention is not limited thereto, and it should be apparent to those skilled in the art that any changes or substitutions that fall within the technical scope of the present invention disclosed herein are within the scope of the present invention.
Claims (10)
1. The cooling and purifying device for the isocyanate carbonylation intermediate is characterized by comprising a barrel, wherein the bottom of the barrel is of a conical structure, a liquid outlet is arranged at the position, close to the tip, of the conical structure, and the barrel is internally divided into a spray granulation area and a liquid phase washing area along the trend of materials in sequence;
the spray granulation zone comprises a granulation system and a cooling system which are sequentially arranged along the trend of the material, and an exhaust port is arranged on the side wall of the cylinder between the granulation system and the cooling system;
the liquid phase washing zone comprises a stirring system and an air ventilation piece which are sequentially arranged along the trend of the material, an overflow port is arranged on the side wall of the barrel between the stirring system and the air ventilation piece, and the air ventilation piece is arranged in the conical structure and is close to the liquid outlet.
2. The cooling and purifying apparatus according to claim 1, wherein the top of the cylinder is provided with a feed inlet and an air inlet, respectively;
preferably, the granulating system comprises an ejector, a baffling cylinder and a guide cylinder, wherein the ejector is arranged close to the feeding hole, the baffling cylinder is arranged above the guide cylinder, and one end of the guide cylinder, which is far away from the baffling cylinder, is arranged in a liquid phase in the liquid phase washing zone;
Preferably, the ejector is an ejector sleeve, the ejector sleeve comprises an inner pipe and an outer pipe which are sleeved in sequence from inside to outside, the inner pipe is used for passing materials, and the outer pipe is used for passing gas phase;
preferably, the baffle cylinder is an annular baffle cylinder;
preferably, the annular edge of the annular baffle cylinder is fixedly connected with the inner surface of the cylinder body;
preferably, the annular baffle cylinder and the injector are coaxially arranged;
preferably, the guide cylinder comprises an upper guide cylinder and a lower guide cylinder which are sequentially arranged along the trend of the material;
preferably, the upper guide cylinder comprises a large diameter end and a small diameter end;
preferably, the edge of the large diameter end is fixedly connected with the inner surface of the cylinder, the small diameter end is fixedly connected with the lower guide cylinder, and one end of the lower guide cylinder, which is far away from the upper guide cylinder, is arranged in the liquid phase washing zone;
preferably, the exhaust port is arranged at one side of the cylinder corresponding to the guide upper cylinder;
preferably, the overflow port is disposed at one side of the cylinder corresponding to the guide flow cylinder.
3. The cooling and purifying apparatus according to claim 2, wherein the ejector is provided with at least one;
Preferably, an injection hole is arranged at one end of the injector far away from the feed inlet;
preferably, the top of the baffle cylinder is arranged above the spray hole;
preferably, the diameter of the baffle cylinder is between the diameter of the large diameter end and the diameter of the small diameter end;
preferably, the inner surface of the upper guide cylinder is smooth;
preferably, the roughness of the inner surface of the upper guide cylinder is less than or equal to 0.2 mu m;
preferably, the guide lower cylinder is a straight cylinder;
preferably, the diameter of the lower guide cylinder is 0.5-0.7 times of the maximum diameter of the cylinder.
4. A cooling and purifying apparatus according to claim 2 or 3, wherein the cooling system includes an annular pipe, a spray cooler, and a gas filter, the annular pipe is sleeved at one end of the guide flow cylinder near the guide flow upper cylinder, the spray cooler is disposed on the annular pipe, and the gas filter is disposed below the spray cooler;
preferably, the nozzle of the spray cooler is inclined downwards and faces towards the axis, and is used for cooling the gas and solid particles flowing through the guide lower cylinder;
preferably, the gas filter is disposed on the guide flow down tube;
Preferably, the gas filter has a filtration accuracy of 1 to 10 μm;
preferably, a liquid inlet is arranged on one side of the cylinder body, which is level with the annular pipeline, and the liquid inlet is connected with the annular pipeline through a liquid inlet pipe.
5. The cooling and purifying apparatus according to any one of claims 2 to 4, wherein the stirring system includes a double-layer stirring paddle, a support column, and a stirring motor, one end of the support column is fixedly connected to the double-layer stirring paddle, the other end of the support column penetrates through the liquid outlet to externally connect the stirring motor, and the double-layer stirring paddle is electrically connected to the stirring motor;
preferably, the double-layer stirring paddle is arranged in the guide lower cylinder;
preferably, the double-layer stirring paddle comprises a flat paddle and an anchor paddle which are sequentially arranged along the material trend;
preferably, the anchor paddle is a V-shaped anchor paddle;
preferably, the flat paddle and the anchor paddle are coaxially arranged, and the distance between the flat paddle and the anchor paddle is 0.16-0.25 times the height of the cylinder.
6. The cooling and purifying apparatus according to any one of claims 1 to 5, wherein the ventilation member is a ventilation cone, and a surface of the ventilation cone is provided with a through hole;
Preferably, the tip of the ventilation cone is arranged corresponding to the tip of the conical structure;
preferably, the through hole is provided with at least one;
preferably, the diameter of the through hole is 1-3 mm;
preferably, an air hole is arranged on the air outlet pipe, and the air hole is used for ventilating the ventilation cone;
preferably, the surface roughness of the cone structure is less than or equal to 0.4 μm.
7. The cooling and purifying apparatus according to any one of claims 2 to 6, wherein the gas inlet is for inert gas intake, and the inert gas is carbon dioxide and nitrogen;
preferably, the feed port is for a crude intermediate feed, and the crude intermediate is a melting point feed;
preferably, the volume ratio of the inert gas to the crude intermediate is (4-10): 1;
preferably, the air inlet temperature of the inert gas is 25-60 ℃;
preferably, the pressure of the inert gas is greater than the pressure of the cooling purification device;
preferably, the pressure difference between the inert gas and the cooling and purifying device is 0.05-0.2 MPa;
preferably, the mass ratio of the spraying amount of the cooling system to the feeding amount of the crude intermediate is (2-4): 1;
preferably, the spray liquid adopted by the cooling system is desalted water or dimethyl carbonate.
8. A cooling and purifying system, characterized in that the cooling and purifying system comprises a cooling and purifying device, a centrifugal device and a melting device which are connected in sequence by pipelines, and the cooling and purifying device adopts the cooling and purifying device as claimed in any one of claims 1 to 7.
9. The cooling and purifying system according to claim 8, wherein the centrifugal device is a centrifuge;
preferably, the centrifugal machine is a two-stage push plate type centrifugal machine;
preferably, the melting device is a melting tank.
10. The cooling and purifying system according to claim 8 or 9, wherein the mass ratio of the amount of the leaching liquid used by the centrifugal device to the material of the feed inlet is (0.5-1): 1;
preferably, the temperature of the melting device is higher than the melting point of the purge material;
preferably, the difference between the temperature of the melting device and the melting point of the purified material is 5-10 ℃;
preferably, the leaching solution adopted by the centrifugal device is desalted water or dimethyl carbonate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310883412.3A CN116747785A (en) | 2023-07-18 | 2023-07-18 | Cooling and purifying device and cooling and purifying system for isocyanate carbonylation intermediate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310883412.3A CN116747785A (en) | 2023-07-18 | 2023-07-18 | Cooling and purifying device and cooling and purifying system for isocyanate carbonylation intermediate |
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| Publication Number | Publication Date |
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| CN116747785A true CN116747785A (en) | 2023-09-15 |
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|---|---|---|---|
| CN202310883412.3A Pending CN116747785A (en) | 2023-07-18 | 2023-07-18 | Cooling and purifying device and cooling and purifying system for isocyanate carbonylation intermediate |
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| Country | Link |
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| CN (1) | CN116747785A (en) |
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