CN210729533U - 1, 5-naphthalene diisocyanate cold reaction reflux unit - Google Patents
1, 5-naphthalene diisocyanate cold reaction reflux unit Download PDFInfo
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- CN210729533U CN210729533U CN201921609622.9U CN201921609622U CN210729533U CN 210729533 U CN210729533 U CN 210729533U CN 201921609622 U CN201921609622 U CN 201921609622U CN 210729533 U CN210729533 U CN 210729533U
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Abstract
The utility model discloses a 1, 5-naphthalene diisocyanate cold reaction reflux unit, including the reation kettle that is provided with the clamp sleeve on the cauldron body, be provided with agitating unit in the internal chamber of cauldron, cauldron body bottom is equipped with liquid nitrogen entry and second feed back mouth, cauldron body inner chamber upper portion is provided with the demister, cauldron body upper portion is provided with gas material export and first feed back mouth, gas material export is communicated to cyclone's feed inlet through the pipeline, cyclone top is equipped with gas outlet, the bottom is equipped with liquid outlet, gas outlet communicates the condenser through the pipeline, condenser upper portion is equipped with the tail gas export, the condenser lower part is equipped with the liquid discharge gate, the liquid discharge gate communicates the second feed back mouth of reation kettle bottom through the pipeline; the liquid outlet at the bottom of the cyclone separator is communicated with the feeding hole of the buffer tank through a pipeline, and the discharging hole of the buffer tank is communicated with the first return port at the upper part of the reaction kettle through a pipeline. The utility model discloses the backward flow is effectual, and the energy consumption is low, can improve the yield and the quality of end product.
Description
Technical Field
The utility model belongs to the technical field of chemical production equipment, concretely relates to cold reaction reflux unit of 1, 5-naphthalene diisocyanate.
Background
1, 5-Naphthalene Diisocyanate (NDI) is a high-performance special isocyanate, and a polyurethane product prepared from the isocyanate has the advantages of high hardness, good rebound resilience, good heat resistance, excellent dynamic performance, good wear resistance and the like, can be used in occasions where ordinary polyurethane cannot meet requirements or is damaged prematurely, such as environments of high temperature, grease and the like, and is widely used as a raw material for synthesizing high-grade polyurethane. In addition, they are also frequently used as agricultural chemicals and pharmaceutical intermediates. The 1, 5-dinaphthyl isocyanate product has the advantages of high melting point, excellent elasticity, good dynamic performance, long service life and the like, so the application prospect is very wide. In the existing production method of 1, 5-naphthalene diisocyanate, a primary cooling cold reaction reflux process and a primary heating and warming hot reaction reflux process are required to be carried out in the synthesis process, wherein the cold reaction mainly comprises the steps of forming 1, 5-dicarbamoyl chloride by using 1, 5-diaminonaphthalene and bis (trichloromethyl) carbonate as raw materials, the hot reaction is the pyrolysis of the 1, 5-dicarbamoyl chloride to form a final product 1, 5-naphthalene diisocyanate, the reflux is required in both reactions, one of the two reactions aims is to ensure that a system solvent cannot be lost due to gas entrainment, so that the material concentration of the system is changed, and the other one is to recycle a low-boiling-point intermediate to return to the system to continuously participate in the reaction; the two reaction processes are respectively very important for the quality and the yield of the product, but in the prior art, the reaction reflux is carried out only by adopting a mode of cooling a reaction kettle jacket and then condensing by a condenser for reflux, so that the cold reaction efficiency is low, the temperature control is higher, the reaction time is long, the side reactions are more, the utilization rate of raw materials is low, the product quality is poor, the yield is low, the load of tail gas treatment is increased, and the total cost is higher.
Disclosure of Invention
The utility model discloses the technical problem that will solve is: aiming at the defects in the prior art, the 1, 5-naphthalene diisocyanate cold reaction reflux device can solve the problems of poor reflux effect, low product yield, poor quality and the like.
In order to solve the technical problem, the technical scheme of the utility model is that:
a1, 5-naphthalene diisocyanate cold reaction reflux device comprises a reaction kettle, wherein a jacket is arranged on a kettle body, a stirring device is arranged in an inner cavity of the kettle body, a liquid nitrogen inlet and a second feed back hole are formed in the bottom of the kettle body, a demister is arranged at the upper part of the inner cavity of the kettle body, a gas material outlet and a first feed back hole are formed in the upper part of the kettle body, the gas material outlet is communicated with a feed inlet of a cyclone separator through a pipeline, a gas outlet is formed in the top of the cyclone separator, a liquid outlet is formed in the bottom of the cyclone separator, the gas outlet is communicated with a condenser through a pipeline, a tail gas outlet is formed in the upper part of the condenser, a liquid discharge hole is formed in; the liquid outlet at the bottom of the cyclone separator is communicated with the feeding hole of the buffer tank through a pipeline, and the discharging hole of the buffer tank is communicated with the first return port at the upper part of the reaction kettle through a pipeline.
Preferably, the reaction kettle is an enamel reaction kettle. Because the system generates acid media such as hydrogen chloride, the enamel reaction kettle is preferred
Preferably, the demister is an enamel grid demister. Because after letting in the liquid nitrogen, the liquid nitrogen vaporization absorbs a large amount of heat to produce a large amount of gas and product and mix and have a large amount of bubbles, if these bubbles do not pass through the elimination, can break after getting into the pipeline and adhere to the pipe wall with the reactant, and the slow siltation can block up the pipeline, adopts the demister can solve this problem.
Preferably, the cyclone separator is QLXF-5.5
A production factory of the cyclone separator is a green-starting environmental protection technology company Limited in Dongguan city. The cyclone separator can perform gas-liquid separation, and the liquid is thrown to the wall andthe gas falls down due to gravity and enters the buffer tank through the second liquid discharge port, and the gas enters the condenser through the gas outlet.
Preferably, the condenser is a YKC40-10 type round block hole graphite heat exchanger, and the manufacturer is Nantong graphite equipment manufacturer. And further separating the separated gas, cooling the solvent and the low-boiling-point carbonyl chloride carried by the gas, returning the cooled gas to the kettle, and continuing to participate in the reaction.
Preferably, the tail gas outlet of the condenser is communicated with a tail gas absorption device through a pipeline.
Preferably, a U-shaped pipeline area is arranged on a pipeline between the buffer tank and the reaction kettle, and the U-shaped pipe plays a role of liquid seal and prevents gas from flowing back into the reaction kettle.
Preferably, a U-shaped pipeline area is arranged on a pipeline between the condenser and the reaction kettle, and the U-shaped pipeline plays a role of liquid seal and prevents gas from flowing back into the reaction kettle.
Since the technical scheme is used, the beneficial effects of the utility model are that:
the utility model adopts liquid nitrogen as direct refrigerant, one of which can be rapidly cooled, ensures the system temperature to be carried out at low temperature (-10 ℃), ensures the nitrogen generated by the second can carry the hydrogen chloride generated by the reaction to rapidly leave the reaction system, accelerates the reaction to be carried out, shortens the reaction time, and can play an auxiliary stirring effect, because the system is carried out at low temperature, the material system has a little viscosity, the nitrogen is dispersed and escaped from the bottom to play an auxiliary stirring effect, and the reaction is accelerated to be carried out; due to the generation of a large amount of gas in the system, the foam formed by materials carried by rising gas can be broken by the grid demister, and the foam is adhered to the wall of a rising pipe or enters a condenser to cause blockage; the reason for replacing the conventional condenser with the cyclone separator is that the gas flow rate is high, the efficiency of the conventional condenser is too low, and the cyclone separator not only can play a role in reducing the speed of the gas flow, but also can perform gas-liquid separation. Buffer tank and U-shaped pipeline all play the effect of liquid seal, and the condenser of this application plays the solvent of grabbing back gas and smuggleing back gas secretly and low boiling point phosgene backward flow to reation kettle in, continue to participate in the reaction.
In a word, the utility model discloses it is effectual to flow back, and the energy consumption is low, can improve the yield and the quality of end product.
Drawings
FIG. 1 is a schematic flow diagram of an apparatus according to an embodiment of the present invention;
in the figure, 1-a reaction kettle; 2-a jacket; 3-a stirring device; 4-liquid nitrogen inlet; 5-a second feed back port; 6-a demister; 7-gas material outlet; 8-a first feed back port; 9-a cyclone separator; 10-a condenser; 11-a buffer tank; 12- "U" shaped pipeline region.
Detailed Description
The invention is further explained below with reference to the drawings and examples.
The first embodiment is as follows:
as shown in fig. 1, a 1, 5-naphthalene diisocyanate cold reaction reflux device comprises a reaction kettle 1 provided with a jacket 2 on a kettle body, a stirring device 3 is arranged in an inner cavity of the kettle body, a liquid nitrogen inlet 4 and a second feed back port 5 are arranged at the bottom of the kettle body, a demister 6 is arranged at the upper part of the inner cavity of the kettle body, a gas material outlet 7 and a first feed back port 8 are arranged at the upper part of the kettle body, the gas material outlet 7 is communicated with a feed inlet (not marked) of a cyclone separator 9 through a pipeline, a gas outlet (not marked) is arranged at the top of the cyclone separator 9, a liquid outlet (not marked) is arranged at the bottom of the cyclone separator, the gas outlet is communicated with a condenser 10 through a pipeline, a tail gas outlet (not marked) is arranged at the upper part of the condenser 10, a liquid discharge port (not marked) is arranged at the; the liquid outlet at the bottom of the cyclone separator 9 is communicated with the feed inlet (not marked) of the buffer tank 11 through a pipeline, and the discharge outlet (not marked) of the buffer tank 11 is communicated with the first return port 8 at the upper part of the reaction kettle 1 through a pipeline.
A U-shaped pipeline area 12 is arranged on a pipeline between the buffer tank 11 and the reaction kettle 1; the pipeline between the condenser 10 and the reaction kettle 1 is provided with a U-shaped pipeline area 12.
The specific use example is as follows:
5 to 25 percent of organic amine inert organic solution is dripped into the inert organic solution of bis (trichloromethyl) carbonate with the mass percentage concentration of 5 to 50 percent in a reaction kettle 1 with a stirring device 3 and a jacket 2, liquid nitrogen is introduced, the flow rate is controlled, the temperature in the kettle is controlled at minus 10 to 10 ℃, and the activation reaction is carried out for 0.5 to 1 hour. The process comprises the steps of forming 1, 5-diamino formyl chloride and hydrogen chloride gas, enabling the nitrogen gas and the hydrogen chloride gas to enter a cyclone separator 9 for first gas-liquid separation, throwing out liquid (with the temperature of about-10 ℃) and falling into a buffer tank 11, and then refluxing the liquid into a reaction kettle 1 through the buffer tank 11; the gas separated by the cyclone separator 9 enters a condenser 10 for further gas-liquid separation, the temperature of the liquid obtained after condensation is approximately-10-0 ℃, the liquid flows back into the reaction kettle 1 through a second feed back port 5 positioned at the bottom of the reaction kettle 1, and the reaction is continued; the tail gas containing gases such as nitrogen, hydrogen chloride and the like enters a tail gas absorption device for treatment.
The device system shortens synthetic time of cold reaction about 1/3 ~ 1/2, has improved production efficiency by a wide margin, and the device carries out secondary gas-liquid separation, has retrieved solvent and intermediate product and has returned the production and use, and utilization ratio of raw materials improves about 10%, and tail gas treatment cost has reduced about 10%, and the yield of product has improved about 3 ~ 5%.
It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Furthermore, it should be understood that various changes and modifications of the present invention may be made by those skilled in the art after reading the teachings of the present invention, and these equivalents also fall within the scope of the appended claims.
Claims (7)
1. The utility model provides a cold reaction reflux unit of 1, 5-naphthalene diisocyanate, is provided with the reation kettle who presss from both sides the cover on the cauldron body, is equipped with agitating unit in the internal chamber of cauldron, its characterized in that: the bottom of the kettle body is provided with a liquid nitrogen inlet and a second return port, the upper part of an inner cavity of the kettle body is provided with a demister, and the upper part of the kettle body is provided with a gas material outlet and a first return port; the gas material outlet is communicated with a feed inlet of the cyclone separator through a pipeline, the top of the cyclone separator is provided with a gas outlet, and the bottom of the cyclone separator is provided with a liquid outlet; the gas outlet is communicated with a condenser through a pipeline, the upper part of the condenser is provided with a tail gas outlet, and the lower part of the condenser is provided with a liquid discharge hole; the liquid discharge port is communicated to a second feed back port at the bottom of the reaction kettle through a pipeline; and a liquid outlet at the bottom of the cyclone separator is communicated with a feed inlet of the buffer tank through a pipeline, and a discharge outlet of the buffer tank is communicated with a first return port at the upper part of the reaction kettle through a pipeline.
2. The cold reaction reflux apparatus of 1, 5-naphthalene diisocyanate according to claim 1, wherein: the reaction kettle is an enamel reaction kettle.
3. The cold reaction reflux apparatus of 1, 5-naphthalene diisocyanate according to claim 1, wherein: the demister is an enamel grid demister.
4. The cold reaction reflux apparatus of 1, 5-naphthalene diisocyanate according to claim 1, wherein: the cyclone separator is QLXF-5.5
A cyclone separator.
5. The cold reaction reflux apparatus of 1, 5-naphthalene diisocyanate according to claim 1, wherein: the condenser is a YKC40-10 type round block hole type graphite heat exchanger.
6. The cold reaction reflux apparatus of 1, 5-naphthalene diisocyanate according to claim 1, wherein: and a tail gas outlet of the condenser is communicated to a tail gas absorption device through a pipeline.
7. The cold reaction reflux apparatus of 1, 5-naphthalene diisocyanate according to claim 1, wherein: the pipeline between buffer tank and reation kettle is provided with "U" shape pipeline district, the pipeline between condenser and the reation kettle is provided with "U" shape pipeline district.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201921609622.9U CN210729533U (en) | 2019-09-24 | 2019-09-24 | 1, 5-naphthalene diisocyanate cold reaction reflux unit |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201921609622.9U CN210729533U (en) | 2019-09-24 | 2019-09-24 | 1, 5-naphthalene diisocyanate cold reaction reflux unit |
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| CN210729533U true CN210729533U (en) | 2020-06-12 |
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| CN201921609622.9U Active CN210729533U (en) | 2019-09-24 | 2019-09-24 | 1, 5-naphthalene diisocyanate cold reaction reflux unit |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112742334A (en) * | 2020-12-14 | 2021-05-04 | 湖南福千府生物科技有限公司 | Sodium sulfite preparation is with raw materials device that mixes equally |
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2019
- 2019-09-24 CN CN201921609622.9U patent/CN210729533U/en active Active
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112742334A (en) * | 2020-12-14 | 2021-05-04 | 湖南福千府生物科技有限公司 | Sodium sulfite preparation is with raw materials device that mixes equally |
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