CN102976976A - Preparation method for methyl isocyanate - Google Patents
Preparation method for methyl isocyanate Download PDFInfo
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- CN102976976A CN102976976A CN2012104980847A CN201210498084A CN102976976A CN 102976976 A CN102976976 A CN 102976976A CN 2012104980847 A CN2012104980847 A CN 2012104980847A CN 201210498084 A CN201210498084 A CN 201210498084A CN 102976976 A CN102976976 A CN 102976976A
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Abstract
The invention discloses a preparation method for methyl isocyanate (iso-ester for short), comprising the following steps of: mixing methylaminoformyl chloride with a non-ozone-depleting substance (ODS) trichloromethane solvent to form a 15-25% methylaminoformyl/trichloromethane organic solution; continuously decomposing via a decomposer; performing product and solvent separation on the decomposition solution via a cyclone-type steam-liquid separator; and rectifying via a coarse esterification tower and a fine esterification tower to obtain methyl isocyanate having a purity of greater than 99%. The reaction equation is shown in the specification; and in the preparation method disclosed by the invention, with the adoption of a process taking the non-ODS substance, namely, trichloromethane, as the solvent of the decomposition reaction, and with the adoption of the cyclone-type steam-liquid separator, ODS substances with damages on environment, such as benzene, methylbenzene and chlorobenzene, are replaced, and the key technological problem of hardness to separate gas and solution due to the boiling point depression of the non-ODS solvent is solved. The produced methyl isocyanate is high in product yield of greater than 93% and high in product purity of greater than 99%, thus meeting requirements on the circular economy development of the modern chemical industry.
Description
Technical field
The present invention relates to the organic chemical synthesis field, particularly a kind of preparation method of methyl isocyanate.
Background technology
Methyl isocyanate is a kind of important pesticide intermediate, be mainly used in synthesis of carbamates class agricultural chemicals, such as: carbofuran, methomyl, meta-tolyl-N-methylcarbamate (MTMC), isoprocarb (Ro 7-5050), fenobucarb (Ba Sha), carbaryl, Propoxur, pacify prestige, UC-51762, benfuracarb, tebuthiuron etc. well.
Mostly adopt in the methyl isocyanate producing country at present take phosgene and methylamine as raw material and prepare methyl amido formyl chloride, then in the presence of the inert solvent tetracol phenixin, methyl amido formyl chloride decomposes, methyl isocyanate is produced in rectifying, product yield 85~90%(molar fraction), product purity 97~99%(massfraction).The decomposition reaction solvent tetracol phenixin that the existing production technique of methyl isocyanate is used belongs to the material that damages the ozone layer (being called for short the ODS material), is the kind that the Montreal protocol regulation must be eliminated.Methyl isocyanate concerns the life-and-death lifeblood of industry as most important intermediate in the carbamate chemicals for agriculture industry, therefore, must carry out the methyl isocyanate production technique and improve, and substitutes existing ODS material tetracol phenixin with non-ODS material.
Non-ODS solvent is more, low according to economy and the most boiling point of technical alternative non-ODS material, acyl chlorides decomposed solution product and separated from solvent are difficult, must be by adopting suitable gas-liquid separation technology, the gordian technique difficult problem that the gas-liquid that solution causes because non-ODS solvent boiling point reduces is difficult to separate.
Summary of the invention
The preparation method of methyl isocyanate provided by the invention (being called for short different ester), it is characterized in that methyl amido formyl chloride is become concentration with the non-material that damages the ozone layer (being called for short non-ODS material) trichloromethane solvent is 15~25%(massfraction) methyl amido formyl chloride/trichloromethane organic solution (be called for short MCC-CHCl
3), methyl amido formyl chloride/trichloromethane organic solution is carried out the continuous decomposition reaction by splitter, decomposed solution is carried out product and separated from solvent by cyclone type vapour-liquid separator, makes purity greater than the 99%(massfraction through thick ester tower, the rectifying of smart ester tower again) methyl isocyanate.The methyl isocyanate product yield of the present invention's preparation is greater than the 93%(molar fraction).
Reaction equation is as follows:
Concrete technology step of the present invention is as follows:
In mixing tank methyl amido formyl chloride being mixed with mass concentration with non-ODS material trichloromethane solvent is 15~25% MCC-CHCl
3Organic solution is squeezed into header tank and is joined in the splitter again, and the control decomposition temperature is at 46~75 ℃, and the splitter temperature adds MCC-CHCl during to the solvent start vaporizer more continuously
3Organic solution, decomposed solution enter the gas-liquid separation of carrying out product and solvent in the cyclone type vapour-liquid separator, and gas phase enters thick ester tower after condenser cooling, and liquid phase is returned the MCC still that is mixed with the still liquid of thick ester tower and smart ester tower.
Thick ester tower is the continuous still battery tower, the gas phase cooling fluid of vapour liquid separator is from thick ester tower intermediate feed, input speed and kettle base solution rate of yield are in a basic balance, control overhead product extraction temperature, reflux ratio, thick ester column overhead distillate enters smart ester tower through the condenser cooling, different ester crude product returns condenser through the cold-trap of deep cooling tank in the tail gas, and all the other advance exhaust treatment system; Still liquid returns the MCC still that is mixed after treatment.Thick ester column overhead extraction temperature is 38~60 ℃, 62~70 ℃ of tower reactor temperature, and the mole reflux ratio is 9:1~12:1.
Smart ester tower is continuous rectifying tower, thick ester column overhead distillate is from smart ester tower intermediate feed, input speed and kettle base solution rate of yield are in a basic balance, control overhead product extraction temperature, tower reactor temperature, reflux ratio, still liquid returns the MCC still that is mixed after treatment, and overhead extraction liquid obtains the finished product methyl isocyanate through the condenser cooling and advances smart ester tundish.Analyze with chemical method or chromatography, recording the methyl isocyanate product purity is the 99%(massfraction) more than.Product returns condenser through the cold-trap of different ester deep cooling tank in the smart ester tower tail gas, and all the other advance exhaust treatment system.Smart ester column overhead extraction temperature is 38~50 ℃, 60~65 ℃ of tower reactor temperature, and the mole reflux ratio is 4:1~7:1.
Cyclone type vapour-liquid separator is comprised of material inlet, straight tube pipe, gaseous phase outlet, pipe core, guide vane, drop entrapment plate, foam removal silk screen, tapered tube, liquid-phase outlet, the pipe core upper end diameter is 1.2~1.5 times of lower end diameter, thereby make pipe core lower end air pressure be slightly larger than upper end air pressure, be conducive to gaseous component and successfully overflow; Guide vane is installed between straight tube pipe and the pipe core in the shape of a spiral, and the inclination angle is 40~60 °; The drop entrapment plate adopts guide flow type porous stainless steel board to make, and the aperture of pod apertures is Φ 5~10mm, and the pod apertures between centers is 10~20mm; The foam removal silk screen adopts tetrafluoroethylene or polypropylene material to make; Liquid phase component in the high speed rotating air-flow is thrown toward the drop entrapment plate under centrifugal action, and under the effect of gravity and guide flow type orifice plate, flow to the back side of drop entrapment plate, effective like this drop that prevents is with to gas phase again by turbulent flow, thereby improves the efficient of separating, and improves the purity of product; The tapered tube upper end diameter is 2~5 times of lower end diameter, and length is 2~5 times of upper end diameter.
The material inlet of cyclone type vapour-liquid separator is installed in about 3/4 eminence of straight tube pipe, the end sealing of straight tube pipe, guide vane is connected with material inlet, and the guide vane lower end is positioned at about 1/4 eminence of straight tube pipe, and the similar that guide vane and straight tube pipe and pipe core form is in the spiral tube of sealing.
It is decomposition reaction solvent process and cyclone type vapour-liquid separator product separation and solvent that the present invention adopts non-ODS material trichloromethane, substituted the benzene that adopts welding in the existing technique, toluene, the ODS materials such as chlorobenzene, the gordian technique difficult problem that solution is difficult to separate because of the acyl chlorides decomposed solution product that adopts non-ODS solvent boiling point to reduce to cause and solvent gas-liquid, the methyl isocyanate product yield of producing is high, product purity is high, product yield is greater than the 93%(molar fraction), product purity is greater than the 99%(massfraction), satisfy the requirement of modern chemical industry industry recycling economy development.
Description of drawings
Fig. 1 is methyl isocyanate preparation technology flow diagram.
Fig. 2 is cyclone type vapour-liquid cyclone separator arrangement synoptic diagram.
Embodiment
The invention will be further described below in conjunction with embodiment and Figure of description.
Cyclone type vapour-liquid separator shown in Figure 2 is comprised of material inlet 1, straight tube pipe 2, gaseous phase outlet 3, pipe core 4, guide vane 5, drop entrapment plate 6, foam removal silk screen 7, tapered tube 8, liquid-phase outlet 9.Material inlet 1 is installed in straight tube pipe 2 about 3/4 eminences, the end sealing of straight tube pipe 2.Guide vane 5 is connected with material inlet 1, and guide vane 5 lower ends are positioned at straight tube pipe 2 about 1/4 eminences, and the similar that guide vane 5 and straight tube pipe 2 and pipe core 4 form is in the spiral tube of sealing.Pipe core 4 is installed in the center of straight tube pipe 2, and its bottom is positioned at straight tube pipe 2 about 1/2 eminences, and stretch out from the top of straight tube pipe 2 on top, and the top is gaseous phase outlet 3.Foam removal silk screen 7 is installed in the bottom of pipe core 4.Drop entrapment plate 6 is cylindric, is installed in the bottom of straight tube pipe 2, and the upper end is concordant with the lower end of guide vane 5, and the lower end is concordant with the lower end of straight tube pipe 2, and drop entrapment plate 6 walls are the diameter of straight tube pipe 2 apart from straight tube pipe 2 walls 1/15~1/10D(D).Tapered tube 8 tops are connected with straight tube pipe 2 bottoms, and its bottom is liquid-phase outlet 9.
Pipe core 4 upper end diameter are 1.2~1.5 times of lower end diameter, thereby make pipe core lower end air pressure be slightly larger than upper end air pressure, are conducive to gaseous component and successfully overflow; Guide vane 5 is installed between straight tube pipe 2 and the pipe core 4 in the shape of a spiral, and the inclination angle is 40~60 °, preferred 45~50 °; Drop entrapment plate 6 adopts guide flow type porous stainless steel board to make, and the aperture of pod apertures is Φ 5~10mm, and the pod apertures between centers is 10~20mm; Foam removal silk screen 7 adopts tetrafluoroethylene or polypropylene material to make; Liquid phase component in the high speed rotating air-flow is thrown toward drop entrapment plate 6 under centrifugal action, and under the effect of gravity and guide flow type orifice plate, flow to the back side of drop entrapment plate 6, effective like this drop that prevents is with to gas phase again by turbulent flow, thereby improves the efficient of separating, and improves the purity of product; Tapered tube 8 upper end diameter are 2~5 times of lower end diameter, and length is 2~5 times of upper end diameter.
The reaction decomposes liquid of splitter enters straight tube pipe 2 from cyclone type vapour-liquid separator material inlet 1, material generation high speed rotating carries out the liquid phase separation under the guiding of guide vane 5, liquid phase component in the high speed rotating air-flow is thrown toward drop entrapment plate 6 under centrifugal action, and under the effect of gravity and guide flow type orifice plate, flow to the back side of drop entrapment plate 6, prevent that drop is with to gas phase again by turbulent flow.The drop entrapment plate 6 that the lower end of straight tube pipe 2 arranges prevents that drop from splashing and produces the liquid foam that the foam removal silk screen 7 of the lower end setting of pipe core 4 prevents that the liquid foam from entering gas phase when getting rid of to barrel.All liquid phases are returned the MCC still that is mixed through tapered tube 8 from liquid-phase outlet 9, and gas phase is overflowed from gaseous phase outlet 3 through pipe core 4.
Embodiment 1
As shown in Figure 1, with the MCC-CHCl for preparing in the mixing tank
3Organic solution is squeezed into after filtering header tank and is joined and carry out decomposition reaction in the splitter, and the splitter temperature adds MCC-CHCl during to the solvent start vaporizer more continuously
3Organic solution is carried out the continuous decomposition reaction, decomposed solution enters the gas-liquid separation of carrying out product and solvent in the cyclone type vapour-liquid separator, cyclone type vapour-liquid separator gas phase out enters thick ester tower after the condenser cooling, thick ester column overhead distillate enters smart ester tower after the condenser cooling, the tail gas of thick ester tower returns condenser through the different ester crude product of deep cooling tank cold-trap, and all the other advance exhaust treatment system.Smart ester column overhead Produced Liquid obtains the finished product methyl isocyanate through the condenser cooling, and product advances smart ester tundish, for synthetic derived product is laid in.Smart ester tower tail gas returns condenser through different ester deep cooling tank cold-trap product, and all the other advance exhaust treatment system.The still liquid of thick ester tower and smart ester tower all returns the MCC still that is mixed.
In mixing tank methyl amido formyl chloride being mixed with mass concentration with non-ODS material trichloromethane solvent is 15% MCC-CHCl
3Organic solution is squeezed into header tank and is joined and carry out decomposition reaction in the splitter, and the control decomposition temperature is at 65 ℃, and the splitter temperature adds MCC-CHCl during to the solvent start vaporizer more continuously
3Organic solution, decomposed solution enters the cyclone type vapour liquid separator from material inlet 1 as shown in Figure 2, material generation high speed rotating under the guiding of guide vane 5, thereby realization gas-liquid separation, gas phase is overflowed from gaseous phase outlet 3 and enter thick ester tower after the condenser cooling through pipe core 4, the lower end of pipe core 4 is provided with foam removal silk screen 7 and enters gas phase to prevent the liquid foam, be that the streams exit of high speed rotating is provided with drop entrapment plate 6 and prevents that drop from splashing produce the liquid foam when getting rid of to barrel in the lower end of straight tube pipe 2, liquid phase is returned the MCC still that is mixed through tapered tube 8 from liquid-phase outlet 9.
Thick ester tower is the continuous still battery tower, and the gas phase cooling fluid of vapour-liquid separator is from thick ester tower intermediate feed, and input speed and kettle base solution rate of yield are in a basic balance, and thick ester column overhead extraction temperature is 50 ℃, and 62 ℃ of tower reactor temperature, reflux ratio are 9:1.Thick ester column overhead distillate enters smart ester tower through the condenser cooling, and different ester crude product returns condenser through the cold-trap of deep cooling tank in the tail gas, and tail gas advances treatment system; Still liquid returns splitter after treatment.
Smart ester tower is continuous rectifying tower, and thick ester column overhead distillate is from smart ester tower intermediate feed, and input speed and kettle base solution rate of yield are in a basic balance, and smart ester column overhead extraction temperature is 40 ℃, the tower reactor temperature 60 C, and reflux ratio is 4:1.Still liquid returns splitter after treatment, and overhead extraction liquid obtains the finished product methyl isocyanate through the condenser cooling.Product returns condenser through the cold-trap of different ester deep cooling tank in the tail gas, and tail gas advances treatment system.Analyze with chemical method or chromatography, recording the methyl isocyanate product yield is the 94.2%(molar fraction), purity is the 99.4%(massfraction).Purity is the 99%(massfraction) more than.
Embodiment 2
In mixing tank methyl amido formyl chloride being mixed with mass concentration with non-ODS material trichloromethane solvent is 25% MCC-CHCl
3Organic solution is squeezed into header tank and is joined in the splitter again, and the control decomposition temperature is at 75 ℃, and the splitter temperature adds MCC-CHCl during to the solvent start vaporizer more continuously
3Organic solution, decomposed solution enters the cyclone type vapour liquid separator from material inlet 1 as shown in Figure 2, material generation high speed rotating under the guiding of guide vane 5, thereby realization gas-liquid separation, gas phase is overflowed from gaseous phase outlet 3 and enter thick ester tower after the condenser cooling through pipe core 4, the lower end of pipe core 4 is provided with foam removal silk screen 7 and enters gas phase to prevent the liquid foam, be that the streams exit of high speed rotating is provided with drop entrapment plate 6 and prevents that drop from splashing produce the liquid foam when getting rid of to barrel in the lower end of straight tube pipe 2, liquid phase is returned the MCC still that is mixed through tapered tube 8 from liquid-phase outlet 9.
Thick ester tower is the continuous still battery tower, and the gas phase cooling fluid of vapour liquid separator is from thick ester tower intermediate feed, and input speed and kettle base solution rate of yield are in a basic balance, and thick ester column overhead extraction temperature is 38 ℃, the tower reactor temperature 70 C, and reflux ratio is 12:1.Thick ester column overhead distillate enters smart ester tower through the condenser cooling, and different ester crude product returns condenser through the cold-trap of deep cooling tank in the tail gas, and tail gas advances treatment system; Still liquid returns splitter after treatment.
Smart ester tower is continuous rectifying tower, and thick ester column overhead distillate is from smart ester tower intermediate feed, and input speed and kettle base solution rate of yield are in a basic balance, and smart ester column overhead extraction temperature is 38 ℃, and 65 ℃ of tower reactor temperature, reflux ratio are 5:1.Still liquid returns splitter after treatment, and overhead extraction liquid obtains the finished product methyl isocyanate through the condenser cooling.Product returns condenser through the cold-trap of different ester deep cooling tank in the tail gas, and tail gas advances treatment system.Analyze with chemical method or chromatography, recording the methyl isocyanate product yield is the 93.2%(molar fraction), purity is the 99.5%(massfraction).
In mixing tank methyl amido formyl chloride being mixed with mass concentration with non-ODS material trichloromethane solvent is 20% MCC-CHCl
3Organic solution is squeezed into header tank and is joined in the splitter again, and the control decomposition temperature is at 65 ℃, and the splitter temperature adds MCC-CHCl during to the solvent start vaporizer more continuously
3Organic solution, decomposed solution enters the cyclone type vapour liquid separator from material inlet 1 as shown in Figure 2, material generation high speed rotating under the guiding of guide vane 5, thereby realization gas-liquid separation, gas phase is overflowed from gaseous phase outlet 3 and enter thick ester tower after the condenser cooling through pipe core 4, the lower end of pipe core 4 is provided with foam removal silk screen 7 and enters gas phase to prevent the liquid foam, be that the streams exit of high speed rotating is provided with drop entrapment plate 6 and prevents that drop from splashing produce the liquid foam when getting rid of to barrel in the lower end of straight tube pipe 2, liquid phase is returned the MCC still that is mixed through tapered tube 8 from liquid-phase outlet 9.
Thick ester tower is the continuous still battery tower, and the gas phase cooling fluid of vapour liquid separator is from thick ester tower intermediate feed, and input speed and kettle base solution rate of yield are in a basic balance, and thick ester column overhead extraction temperature is 60 ℃, the tower reactor temperature 70 C, and reflux ratio is 10:1.Thick ester column overhead distillate enters smart ester tower through the condenser cooling, and different ester crude product returns condenser through the cold-trap of deep cooling tank in the tail gas, and tail gas advances treatment system; Still liquid returns splitter after treatment.
Smart ester tower is continuous rectifying tower, and thick ester column overhead distillate is from smart ester tower intermediate feed, and input speed and kettle base solution rate of yield are in a basic balance, and smart ester column overhead extraction temperature is 40 ℃, and 65 ℃ of tower reactor temperature, reflux ratio are 5:1.Still liquid returns splitter after treatment, and overhead extraction liquid obtains the finished product methyl isocyanate through the condenser cooling.Product returns condenser through the cold-trap of different ester deep cooling tank in the tail gas, and tail gas advances treatment system.Analyze with chemical method or chromatography, recording the methyl isocyanate product yield is the 93.3%(molar fraction), purity is the 99.2%(massfraction).
Embodiment 4
In mixing tank methyl amido formyl chloride being mixed with mass concentration with non-ODS material trichloromethane solvent is 20% MCC-CHCl
3Organic solution is squeezed into header tank and is joined in the splitter again, and the control decomposition temperature is at 70 ℃, and the splitter temperature adds MCC-CHCl during to the solvent start vaporizer more continuously
3Organic solution, decomposed solution enters the cyclone type vapour liquid separator from material inlet 1 as shown in Figure 2, material generation high speed rotating under the guiding of guide vane 5, thereby realization gas-liquid separation, gas phase is overflowed from gaseous phase outlet 3 and enter thick ester tower after the condenser cooling through pipe core 4, the lower end of pipe core 4 is provided with foam removal silk screen 7 and enters gas phase to prevent the liquid foam, be that the streams exit of high speed rotating is provided with drop entrapment plate 6 and prevents that drop from splashing produce the liquid foam when getting rid of to barrel in the lower end of straight tube pipe 2, liquid phase is returned the MCC still that is mixed through tapered tube 8 from liquid-phase outlet 9.
Thick ester tower is the continuous still battery tower, and the gas phase cooling fluid of vapour liquid separator is from thick ester tower intermediate feed, and input speed and kettle base solution rate of yield are in a basic balance, and thick ester column overhead extraction temperature is 50 ℃, and 65 ℃ of tower reactor temperature, reflux ratio are 10:1.Thick ester column overhead distillate enters smart ester tower through the condenser cooling, and different ester crude product returns condenser through the cold-trap of deep cooling tank in the tail gas, and tail gas advances treatment system; Still liquid returns splitter after treatment.
Smart ester tower is continuous rectifying tower, and thick ester column overhead distillate is from smart ester tower intermediate feed, and input speed and kettle base solution rate of yield are in a basic balance, and smart ester column overhead extraction temperature is 45 ℃, and 62 ℃ of tower reactor temperature, reflux ratio are 7:1.Still liquid returns splitter after treatment, and overhead extraction liquid obtains the finished product methyl isocyanate through the condenser cooling.Product returns condenser through the cold-trap of different ester deep cooling tank in the tail gas, and tail gas advances treatment system.Analyze with chemical method or chromatography, recording the methyl isocyanate product yield is the 93.7%(molar fraction), purity is the 96.2%(massfraction).
Claims (4)
1. the preparation method of a methyl isocyanate, it is characterized in that methyl amido formyl chloride is become to methyl amido formyl chloride/chloroform organic solution with the non-material chloroform solvent that damages the ozone layer, by decomposer, carry out the continuous decomposition reaction, decomposed solution is carried out product and separated from solvent by cyclone type vapour-liquid separator, through thick ester tower, the rectifying of smart ester tower, make methyl isocyanate again, the methyl isocyanate product purity is greater than the 99%(mass fraction), yield is greater than the 93%(molar fraction)
Reaction equation is as follows:
。
2. the preparation method of a kind of methyl isocyanate according to claim 1, it is characterized in that entering splitter methyl amido formyl chloride/trichloromethane organic solution mass concentration is 15~25%, decomposition temperature is 46~75 ℃; Cyclone type vapour-liquid separator gas phase out enters thick ester tower after the condenser cooling, thick ester column overhead distillate enters smart ester tower after the condenser cooling, methyl isocyanate crude product in the thick ester tower tail gas reclaims through the cold-trap of deep cooling tank, smart ester column overhead Produced Liquid obtains the product methyl isocyanate through the condenser cooling, the methyl isocyanate product reclaims through the cold-trap of deep cooling tank in the smart ester tower tail gas, thick ester column overhead extraction temperature is 38~60 ℃, 62~70 ℃ of tower reactor temperature, the mole reflux ratio is 9:1~12:1; Smart ester column overhead extraction temperature is 38~50 ℃, 60~65 ℃ of tower reactor temperature, and the mole reflux ratio is 4:1~7:1.
3. the preparation method of a kind of methyl isocyanate according to claim 1, it is characterized in that cyclone type vapour-liquid separator is comprised of material inlet (1), straight tube pipe (2), gaseous phase outlet (3), pipe core (4), guide vane (5), drop entrapment plate (6), foam removal silk screen (7), tapered tube (8), liquid-phase outlet (9), pipe core (4) upper end diameter is 1.2~1.5 times of lower end diameter, thereby make pipe core lower end air pressure be slightly larger than upper end air pressure, be conducive to gaseous component and successfully overflow; Guide vane (5) is installed between straight tube pipe (2) and the pipe core (4) in the shape of a spiral, and the inclination angle is 40~60 °; Drop entrapment plate (6) adopts guide flow type porous stainless steel board to make, and the aperture of pod apertures is Φ 5~10mm, and the pod apertures between centers is 10~20mm; Foam removal silk screen (7) adopts tetrafluoroethylene or polypropylene material to make; Liquid phase component in the high speed rotating air-flow is thrown toward drop entrapment plate (6) under centrifugal action, and under the effect of gravity and guide flow type orifice plate, flow to the back side of drop entrapment plate (6), effective like this drop that prevents is with to gas phase again by turbulent flow, thereby improve the efficient of separating, improve the purity of product; Tapered tube (8) upper end diameter is 2~5 times of lower end diameter, and length is 2~5 times of upper end diameter.
4. the preparation method of a kind of methyl isocyanate according to claim 3, the material inlet (1) that it is characterized in that cyclone type vapour-liquid separator is installed in about 3/4 eminence of straight tube pipe (2), the end sealing of straight tube pipe (2), guide vane (5) is connected with material inlet (1), guide vane (5) lower end is positioned at about 1/4 eminence of straight tube pipe (2), and the similar that guide vane (5) and straight tube pipe (2) and pipe core (4) form is in the spiral tube of sealing.
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CN103694190A (en) * | 2013-12-25 | 2014-04-02 | 沙隆达集团公司 | Production method and equipment of methyl isocyanate |
CN104387295A (en) * | 2014-12-12 | 2015-03-04 | 湖南海利高新技术产业集团有限公司 | Preparation method of methyl isocyanate |
CN104557441A (en) * | 2014-12-25 | 2015-04-29 | 湖北沙隆达股份有限公司 | Method for recycling chloroform in process of producing methyl isocyanate |
CN105418459A (en) * | 2015-12-09 | 2016-03-23 | 海利贵溪化工农药有限公司 | Process for producing high yield methyl isocyanate |
CN108689882A (en) * | 2018-04-24 | 2018-10-23 | 江苏蓝丰生物化工股份有限公司 | The synthetic method of t-butylisocyanate |
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CN103694190A (en) * | 2013-12-25 | 2014-04-02 | 沙隆达集团公司 | Production method and equipment of methyl isocyanate |
CN104387295A (en) * | 2014-12-12 | 2015-03-04 | 湖南海利高新技术产业集团有限公司 | Preparation method of methyl isocyanate |
CN104387295B (en) * | 2014-12-12 | 2017-01-25 | 湖南海利高新技术产业集团有限公司 | Preparation method of methyl isocyanate |
CN104557441A (en) * | 2014-12-25 | 2015-04-29 | 湖北沙隆达股份有限公司 | Method for recycling chloroform in process of producing methyl isocyanate |
CN105418459A (en) * | 2015-12-09 | 2016-03-23 | 海利贵溪化工农药有限公司 | Process for producing high yield methyl isocyanate |
CN105418459B (en) * | 2015-12-09 | 2018-02-23 | 海利贵溪化工农药有限公司 | A kind of production technology of high yield methyl isocyanate |
CN108689882A (en) * | 2018-04-24 | 2018-10-23 | 江苏蓝丰生物化工股份有限公司 | The synthetic method of t-butylisocyanate |
CN115057799A (en) * | 2022-07-21 | 2022-09-16 | 湖南海利常德农药化工有限公司 | Method for preventing fenobucarb technical from discoloring |
CN115057799B (en) * | 2022-07-21 | 2023-11-24 | 湖南海利常德农药化工有限公司 | Method for preventing color change of fenobucarb technical |
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