CN111302360B - Cyanogen chloride preparation process for cyanate resin synthesis - Google Patents

Cyanogen chloride preparation process for cyanate resin synthesis Download PDF

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CN111302360B
CN111302360B CN202010313449.9A CN202010313449A CN111302360B CN 111302360 B CN111302360 B CN 111302360B CN 202010313449 A CN202010313449 A CN 202010313449A CN 111302360 B CN111302360 B CN 111302360B
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pipe
bin
liquid
sodium cyanide
reaction
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CN111302360A (en
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朱芝峰
王跃彪
邵家伟
张科明
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Yangzhou Techia Material Co ltd
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Yangzhou Techia Material Co ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01CAMMONIA; CYANOGEN; COMPOUNDS THEREOF
    • C01C3/00Cyanogen; Compounds thereof
    • C01C3/004Halogenides of cyanogen

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Abstract

The invention discloses a cyanogen chloride preparation process for cyanate ester resin synthesis, and a reactor is used in the cyanogen chloride preparation process, the reactor comprises a base, the upper surface of the base is provided with a reaction bin, the bottom end of the reaction bin is provided with a discharge hole, the top end of the reaction bin is provided with a material collecting hole, and the upper surface of the base is also fixedly provided with a first storage bin, a condensation bin, a first material receiving bin, a second storage bin and a second material receiving bin; sodium cyanide aqueous solution is impressed into the spray tube by the infusion standpipe in with first storage silo through the booster pump, by the spray head blowout, the cross setting of spray head, make sodium cyanide aqueous solution atomize completely, and be full of whole reactor, the jet tube is located both sides about the spray tube, make chlorine can be abundant when getting into the reactor contact with sodium cyanide aqueous solution, discharge gate valve and first drain valve's setting, make unreacted sodium cyanide aqueous solution get into the reaction bin again, make sodium cyanide aqueous solution and chlorine react more fully.

Description

Cyanogen chloride preparation process for cyanate resin synthesis
Technical Field
The invention belongs to the technical field of cyanate ester resin synthesis, and particularly relates to a cyanogen chloride preparation process for cyanate ester resin synthesis.
Background
The chlorination process of the cyanate ester resin is to react sodium cyanide aqueous solution with chlorine to generate a cyanogen chloride intermediate, the reaction is violent and rapid, the heat release amount is large, the corrosivity is strong, the existing special polytetrafluoroethylene reaction nozzle has certain advantages in the aspects of high temperature resistance and corrosion resistance, but the reactor has the following more outstanding defects.
The heat transfer performance is poor, the reaction heat can not be exchanged and taken away in time, the color of the wastewater generated by the reaction is blackened, great difficulty is brought to the later-stage wastewater treatment, and the environmental friendliness is poor.
The reaction can not be processed to the precision of full contact reaction of the raw materials, the mixing effect of the sodium cyanide solution and the chlorine gas in the reactor is poor, and the yield is only 60-70%. Residual unreacted chlorine gas can cause adverse effects on the quality of the cyanogen chloride intermediate, residual sodium cyanide solution which is not completely reacted is discharged and enters a wastewater treatment process, the high-concentration cyanide wastewater treatment difficulty is high, the cost is high, and the toxicity is not beneficial to the growth of active bacteria and the wastewater treatment.
Disclosure of Invention
The invention aims to provide a cyanogen chloride preparation process for cyanate ester resin synthesis.
The technical problems to be solved by the invention are as follows:
1. the heat transfer performance is poor, the reaction heat can not be exchanged and taken away in time, the color of the wastewater generated by the reaction is blackened, great difficulty is brought to the later-stage wastewater treatment, and the environmental friendliness is poor.
2. The reaction can not be processed to the precision of full contact reaction of the raw materials, the mixing effect of the sodium cyanide solution and the chlorine gas in the reactor is poor, and the yield is only 60-70%. Residual unreacted chlorine gas can cause adverse effects on the quality of the cyanogen chloride intermediate, residual sodium cyanide solution which is not completely reacted is discharged and enters a wastewater treatment process, the high-concentration cyanide wastewater treatment difficulty is high, the cost is high, and the toxicity is not beneficial to the growth of active bacteria and the wastewater treatment.
The purpose of the invention can be realized by the following technical scheme:
a cyanogen chloride preparation process for cyanate ester resin synthesis comprises the following steps:
step S1: weighing the following raw materials in parts by weight: 10-15 parts of sodium cyanide solution and 7-12 parts of liquid chlorine;
step S2: adding 30 mass percent sodium cyanide solution and water into a stirring kettle, and stirring for 5-10min at the rotation speed of 800-;
step S3: and (4) adding the sodium cyanide aqueous solution with the mass fraction of 15% and the liquid chlorine prepared in the step (S2) into a reactor, and reacting for 5-10min under the conditions that the temperature is 30-50 ℃ and the pH value is 3-4.5 to prepare the cyanogen chloride.
Further, step S3, the reactor includes a base, a reaction chamber is disposed on an upper surface of the base, a discharge port is disposed at a bottom end of the reaction chamber, a material collecting port is disposed at a top end of the reaction chamber, a first liquid guiding tube and a second liquid guiding tube are fixed on two sides of the discharge port, a material collecting tube is fixed on a top end of the material collecting port and is communicated with an interior of the material collecting port, a material collecting ring tube is disposed at an end of the material collecting tube, the first liquid guiding tube is communicated with the interior of the second liquid guiding tube, a first storage chamber, a condensation chamber, a first material receiving chamber, a second storage chamber and a second material receiving chamber are fixed on an upper surface of the base, a first feed port is disposed at a top end of the first storage chamber, a vertical infusion tube is disposed in the first storage chamber, a top end of the vertical infusion tube passes through the first storage chamber and is fixedly connected with the first storage chamber, a booster pump is fixed on the vertical infusion tube and is matched with the vertical tube, a liquid spraying tube is vertically fixed on the top end of the vertical tube, the liquid spraying pipe is communicated with the interior of the vertical liquid conveying pipe, a plurality of rows of liquid spraying heads which are uniformly distributed are fixed on the liquid spraying pipe, a condensation folding pipe is arranged in the condensation bin, one end of the condensation folding pipe is provided with a folding pipe inlet, the other end of the condensation folding pipe is provided with a folding pipe outlet, the folding pipe inlet and the folding pipe outlet are positioned outside the condensation bin, the bottom end of one side of the condensation bin is provided with a water inlet, one end, away from the water inlet, of the upper surface of the condensation bin is provided with a water outlet, the folding pipe inlet is communicated with a second liquid guide pipe, one side of the first material receiving bin is provided with a first material receiving port, the first material receiving port is matched with the folding pipe outlet, the side wall of the second material storage bin is fixed with a heater, the top end of the second material storage bin is fixed with a first air guide pipe, the first air guide pipe is communicated with the interior of the second material storage bin, the second air guide pipe is vertically fixed with the top end of the second air guide pipe, third air guide pipe is fixed on the upper and the lower two sides of the end of the second air guide pipe, the third air duct is communicated with the inside of the second air duct, an air injection pipe is fixed at the end of the third air duct and located inside the reaction bin, a second feed inlet is formed in the second storage bin, a second material receiving port is formed in the top end of the second material receiving groove, and the second material receiving port is matched with the material collecting ring pipe.
Further, reaction storehouse and base between be fixed with four evenly distributed's support column, the inside of discharge gate is equipped with the discharge gate valve, the inside of gathering materials the mouth is equipped with the material collection mouth valve, first catheter is close to the inside first drain valve that is equipped with of one end of discharge gate, second catheter is close to the inside second drain valve that is equipped with of one end of discharge gate.
Furthermore, the top of the collecting ring pipe is provided with a ring pipe inlet, the bottom of the collecting ring pipe is provided with a ring pipe outlet, the ring pipe inlet is communicated with the collecting pipe, and the ring pipe outlet is communicated with the second collecting port.
Further, the hydrojet head be located the inside in reaction storehouse, every row of hydrojet head's number is four, every row of hydrojet head becomes the cross and arranges, the hydrojet pipe is located the inside center department in reaction storehouse, hydrojet pipe and reaction storehouse fixed connection, the material of hydrojet pipe and hydrojet head is polytetrafluoroethylene.
Furthermore, the end of the first material receiving port is provided with a thread, the end of the first material receiving port is connected with a connector in a threaded manner, the end of the folded pipe outlet is provided with a thread, and the folded pipe outlet is connected with the connector in a threaded manner.
Further, the air injection pipe on be fixed with the jet-propelled side pipe of a plurality of relative settings, open a plurality of evenly distributed's air jet on the jet-propelled side pipe, jet-propelled pipe is mutually perpendicular with the spray line, both sides about the spray line is located to the jet-propelled pipe, are equipped with the air-blower on the second air duct.
Further, the specific operation steps of step S3 are as follows:
adding sodium cyanide aqueous solution into a first storage bin from a first feeding hole, adding the liquid chlorine into a second storage bin from a second feeding hole, starting a heater to heat the liquid chlorine, enabling the chlorine to enter a second air duct from a first air duct, starting an air blower and a booster pump, pressing the sodium cyanide aqueous solution in the first storage bin into a liquid spraying pipe from a vertical infusion pipe by the booster pump, spraying out the chlorine by a liquid spraying head, driving the chlorine to enter a third air duct by the air blower, further entering an air spraying pipe, dispersing the chlorine into a side air spraying pipe, spraying out the chlorine by an air spraying opening, enabling the chlorine to be fully contacted with the sodium cyanide aqueous solution when entering a reactor by the air spraying pipe positioned at the upper side and the lower side of the liquid spraying pipe, reacting for 5-10min under the conditions that the temperature is 30-50 ℃ and the pH value is 3-4.5, collecting the atomized sodium cyanide aqueous solution at the bottom of the reaction bin, and starting a discharge port valve and a first liquid guiding valve, the sodium cyanide aqueous solution reenters first storage silo for unreacted sodium cyanide aqueous solution reenters in the reaction bin, after the reaction, close first drain valve and open second drain valve, let in water by the delivery port discharge by the water inlet, the waste water that the reaction produced is cooled down in getting into the condensation through rolling over the pipe import, waste water after the cooling gets into first receiving storehouse in by rolling over the pipe export, open the collecting opening valve, the cyanogen chloride gas that the reaction produced gets into the collecting pipe, and then get into the collecting ring pipe and liquefy, the cyanogen chloride after the liquefaction, get into second receiving opening by the ring pipe export, collect and obtain the cyanogen chloride.
The invention has the beneficial effects that: the invention uses a reactor in the process of preparing cyanogen chloride, the reactor presses the sodium cyanide aqueous solution in a first storage bin into a liquid spray pipe from a vertical liquid conveying pipe through a booster pump, the sodium cyanide aqueous solution is sprayed out from a liquid spray head, the liquid spray head is arranged in a cross way to lead the sodium cyanide aqueous solution to be completely atomized and to be filled in the whole reactor, a blower drives chlorine gas to enter a third air duct and then enter an air injection pipe, the chlorine gas is dispersed into an air injection side pipe and is sprayed out from an air injection port, the air injection pipe is positioned at the upper side and the lower side of the liquid spray pipe to lead the chlorine gas to be fully contacted with the sodium cyanide aqueous solution when entering the reactor, the atomized sodium cyanide aqueous solution is gathered at the bottom of the reaction bin, a discharge port valve and a first liquid guide valve are opened, the sodium cyanide aqueous solution enters the first storage bin again, and lead the unreacted sodium cyanide aqueous solution to enter the reaction bin again, thus leading the sodium cyanide aqueous solution to be more fully reacted with the chlorine gas, after the reaction, close first drain valve and open second drain valve, let in water by the delivery port discharge by the water inlet, waste water that the reaction produced is cooled down in getting into the condensation book pipe by rolling over the import of pipe, waste water after the cooling is by rolling over in the pipe export gets into first receipts feed bin, the setting up of condensation bin makes the fine heat exchange that carries out of waste water that the reaction produced, and then the processing degree of difficulty of the waste water that reduces, open the material collection mouth valve, the cyanogen chloride gas that the reaction produced gets into the collecting pipe, and then get into the collecting pipe and liquefy, the setting up of collecting pipe makes and need not install liquefying plant additional and liquefy gaseous cyanogen chloride, the equipment cost of reduction, cyanogen chloride preparation efficiency has been increased.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic structural diagram of a reactor in a cyanogen chloride preparation process for cyanate ester resin synthesis according to the present invention;
FIG. 2 is a top view of a reactor used in a cyanogen chloride process for cyanate ester resin synthesis according to the present invention;
FIG. 3 is a side view of a reactor used in a cyanogen chloride process for cyanate ester resin synthesis according to the present invention;
FIG. 4 is a schematic view of a portion of the structure of FIG. 1;
FIG. 5 is a schematic view of a portion of the structure of FIG. 1;
FIG. 6 is a side view of a liquid injection tube in the reactor of the present invention;
FIG. 7 is a top view of a gas lance in the reactor of the present invention.
In the figure: 1. a base; 2. a reaction bin; 21. a discharge port; 211. a discharge port valve; 22. a material collecting port; 221. a material collecting port valve; 222. a material collecting pipe; 223. a collecting ring pipe; 2231. a loop pipe inlet; 2232. a loop pipe outlet; 23. a first catheter; 231. a first drain valve; 24. a second catheter; 241. a second drain valve; 25. a support pillar; 3. a first storage bin; 31. a first feed port; 32. a vertical transfusion tube; 33. a booster pump; 34. a liquid spraying pipe; 341. a liquid jet head; 4. a condensation bin; 41. a condensing folded pipe; 411. a folded tube inlet; 412. a folded tube outlet; 42. a water inlet; 43. a water outlet; 5. a first receiving bin; 51. a first material receiving port; 52. a connector; 6. a second storage bin; 61. a heater; 62. a first air duct; 63. a second air duct; 631. a blower; 64. a third air duct; 65. a gas ejector tube; 66. a gas injection side pipe; 661. an air jet; 67. a second feed port; 7. a second material receiving groove; 71. and a second material receiving port.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A preparation process of cyanogen chloride for cyanate resin synthesis comprises the following steps:
step S1: weighing the following raw materials in parts by weight: 10 parts of sodium cyanide solution and 7 parts of liquid chlorine;
step S2: adding 30 mass percent sodium cyanide solution and water into a stirring kettle, and stirring for 10min at the rotating speed of 800r/min and the temperature of 25 ℃ to prepare 15 mass percent sodium cyanide solution;
step S3: and (4) adding the sodium cyanide aqueous solution with the mass fraction of 15% and the liquid chlorine prepared in the step (S2) into a reactor, and reacting for 10min under the conditions that the temperature is 30 ℃ and the pH value is 3 to prepare the cyanogen chloride.
Example 2
A preparation process of cyanogen chloride for cyanate resin synthesis comprises the following steps:
step S1: weighing the following raw materials in parts by weight: 13 parts of sodium cyanide solution and 10 parts of liquid chlorine;
step S2: adding 30 mass percent sodium cyanide solution and water into a stirring kettle, and stirring for 8min at the rotating speed of 900r/min and the temperature of 28 ℃ to prepare 15 mass percent sodium cyanide solution;
step S3: and (4) adding the sodium cyanide aqueous solution with the mass fraction of 15% and the liquid chlorine prepared in the step (S2) into a reactor, and reacting for 8min under the conditions that the temperature is 40 ℃ and the pH value is 4 to prepare the cyanogen chloride.
Example 3
A preparation process of cyanogen chloride for cyanate resin synthesis comprises the following steps:
step S1: weighing the following raw materials in parts by weight: 15 parts of sodium cyanide solution and 12 parts of liquid chlorine;
step S2: adding 30 mass percent sodium cyanide solution and water into a stirring kettle, and stirring for 10min at the rotation speed of 1000r/min and the temperature of 30 ℃ to prepare 15 mass percent sodium cyanide solution;
step S3: and (4) adding the sodium cyanide aqueous solution with the mass fraction of 15% and the liquid chlorine prepared in the step (S2) into a reactor, and reacting for 10min under the conditions that the temperature is 50 ℃ and the pH value is 4.5 to prepare the cyanogen chloride.
Comparative example 1
The comparative example carried out without using a tubular reactor instead of the reactor described in step S3, the specific steps were as follows:
step S1: weighing the following raw materials in parts by weight: 10 parts of sodium cyanide solution and 7 parts of liquid chlorine;
step S2: adding 30 mass percent sodium cyanide solution and water into a stirring kettle, and stirring for 10min at the rotating speed of 800r/min and the temperature of 25 ℃ to prepare 15 mass percent sodium cyanide solution;
step S3: and (4) adding the sodium cyanide aqueous solution with the mass fraction of 15% and the liquid chlorine prepared in the step (S2) into a tubular reactor, and reacting for 10min under the conditions that the temperature is 30 ℃ and the pH value is 3 to prepare the cyanogen chloride.
Cyanogen chloride prepared in examples 1 to 3 and comparative example 1 was subjected to content measurement, and wastewater generated from the reaction was examined, and the examination results are shown in table 1 below;
TABLE 1
Example 1 Example 2 Example 3 Comparative example 1
Cyanogen chloride content 98.32% 99.28% 98.74% 88.51%
CN content in wastewater 60PPM 55PPM 60PPM 230PPM
Color of wastewater Light yellow Light yellow Light yellow Black color
From the above table 1, it can be seen that the cyanogen chloride prepared by the processes of examples 1 to 3 has a cyanogen chloride content of 98.32% to 99.28%, a CN content of 55PPM in the produced wastewater, and a pale yellow color in the wastewater, which indicates that the cyanogen chloride preparation process for cyanate ester resin synthesis of the present invention has a higher chlorination yield and less pollution compared with the conventional process.
Referring to fig. 1-7, the reactor used in the above embodiment includes a base 1, a reaction chamber 2 is disposed on the upper surface of the base 1, a discharge port 21 is disposed at the bottom end of the reaction chamber 2, a collection port 22 is disposed at the top end of the reaction chamber 2, a first liquid guide tube 23 and a second liquid guide tube 24 are fixed on two sides of the discharge port 21, a collection tube 222 is fixed on the top end of the collection port 22, the collection tube 222 is communicated with the interior of the collection port 22, a collection ring tube 223 is disposed at the end of the collection tube 222, the first liquid guide tube 23 is communicated with the interior of the second liquid guide tube 24, a first storage chamber 3, a condensation chamber 4, a first storage chamber 5, a second storage chamber 6, and a second storage chamber 7 are further fixed on the upper surface of the base 1, a first feed port 31 is disposed on the top end of the first storage chamber 3, a vertical infusion tube 32 is disposed inside the first storage chamber 3, the vertical infusion tube 32 passes through the first storage chamber 3, and is fixedly connected to the first storage chamber 3, a booster pump 33 is fixed on the vertical infusion tube 32, the booster pump 33 is matched with the vertical infusion tube 32, a liquid spray tube 34 is vertically fixed at the top end of the vertical infusion tube 32, the liquid spray tube 34 is communicated with the interior of the vertical infusion tube 32, a plurality of rows of liquid spray heads 341 which are uniformly distributed are fixed on the liquid spray tube 34, a condensation folding tube 41 is arranged in the condensation bin 4, a folding tube inlet 411 is arranged at one end of the condensation folding tube 41, a folding tube outlet 412 is arranged at the other end of the condensation folding tube 41, the folding tube inlet 411 and the folding tube outlet 412 are positioned outside the condensation bin 4, a water inlet 42 is arranged at the bottom end of one side of the condensation bin 4, a water outlet 43 is arranged at one end, far away from the water inlet 42, the folding tube inlet 411 is communicated with the second liquid guide tube 24, a first material receiving port 51 is arranged at one side of the first material receiving bin 5, the first material receiving port 51 is matched with the folding tube outlet 412, a heater 61 is fixed on the side wall of the second material storage bin 6, the top of second storage silo 6 is fixed with first air duct 62, first air duct 62 and the inside intercommunication of second storage silo 6, the top vertical fixation of first air duct 62 has second air duct 63, second air duct 63 and the inside intercommunication of first air duct 62, both sides are fixed with third air duct 64 about the end of second air duct 63, third air duct 64 and the inside intercommunication of second air duct 63, the end of third air duct 64 is fixed with jet-propelled pipe 65, jet-propelled pipe 65 is located the inside of reaction chamber 2, be equipped with second feed inlet 67 on the second storage silo 6, the top of second receipts silo 7 is equipped with second receipts material mouth 71, second receipts material mouth 71 cooperatees with collection ring pipe 223.
Reaction chamber 2 and base 1 between be fixed with four evenly distributed's support column 25, the inside of discharge gate 21 is equipped with discharge gate valve 211, the inside of gathering materials mouth 22 is equipped with collection mouth valve 221, first catheter 23 is close to the inside first drain valve 231 that is equipped with of one end of discharge gate 21, second catheter 24 is close to the inside second drain valve 241 that is equipped with of one end of discharge gate 21.
The top end of the collecting ring pipe 223 is provided with a ring pipe inlet 2231, the bottom end of the collecting ring pipe 223 is provided with a ring pipe outlet 2232, the ring pipe inlet 2231 is communicated with the collecting pipe 222, and the ring pipe outlet 2232 is communicated with the second material receiving port 71.
The liquid spray heads 341 are located inside the reaction bin 2, the number of the liquid spray heads 341 in each row is four, the liquid spray heads 341 in each row are arranged in a cross shape, the liquid spray pipe 34 is located in the center inside the reaction bin 2, the liquid spray pipe 34 is fixedly connected with the reaction bin 2, and the liquid spray pipe 34 and the liquid spray heads 341 are made of polytetrafluoroethylene.
The end of the first material receiving opening 51 is provided with threads, the end of the first material receiving opening 51 is connected with the connector 52 in a threaded manner, the end of the folded pipe outlet 412 is provided with threads, and the folded pipe outlet 412 is in threaded connection with the connector 52.
The air injection pipe 65 is fixed with a plurality of air injection side pipes 66 which are arranged oppositely, a plurality of air injection ports 661 which are distributed evenly are arranged on the air injection side pipes 66, the air injection pipe 65 is vertical to the liquid injection pipe 34, the air injection pipe 65 is positioned on the upper side and the lower side of the liquid injection pipe 34, and the second air guide pipe 63 is provided with an air blower 631.
The working principle is as follows: adding sodium cyanide aqueous solution into a first storage bin 3 from a first feeding hole 31, adding the liquid chlorine into a second storage bin 6 from a second feeding hole 67, starting a heater 61 to heat the liquid chlorine, enabling the chlorine to enter a second air duct 63 from a first air duct 62, starting a blower 631 and a booster pump 33, enabling the sodium cyanide aqueous solution in the first storage bin 3 to be pressed into a liquid spraying tube 34 from an infusion vertical tube 32 by the booster pump 33, spraying out the chlorine from a liquid spraying head 341, enabling the sodium cyanide aqueous solution to be completely atomized and filling the whole reactor by arranging the liquid spraying head 341 in a cross manner, enabling the chlorine to enter a third air duct 64 by the blower 631, further entering an air spraying tube 65, dispersing the chlorine into an air spraying side tube 66, spraying out 661 from an air spraying opening, enabling the chlorine to be fully contacted with the sodium cyanide aqueous solution when the chlorine enters the reactor by the air spraying tube 65 being positioned at the upper side and the lower side of the liquid spraying tube 34, and under the conditions that the temperature is 30-50 ℃ and the pH value is 3-4.5, reacting for 5-10min, collecting the atomized sodium cyanide aqueous solution at the bottom of the reaction bin 2, opening the discharge port valve 211 and the first liquid guide valve 231, allowing the sodium cyanide aqueous solution to reenter the first storage bin 3, allowing the unreacted sodium cyanide aqueous solution to reenter the reaction bin 2, allowing the sodium cyanide aqueous solution to react with chlorine more fully, after the reaction is finished, closing the first liquid guide valve 231, opening the second liquid guide valve 241, introducing water from the water inlet 42 and discharging the water from the water outlet 43, allowing the wastewater generated by the reaction to enter from the folded tube inlet 411, cooling in the folded condensation tube 41, allowing the cooled wastewater to enter the first collection bin 5 from the folded tube outlet 412, allowing the wastewater generated by the reaction to exchange heat well due to the arrangement of the condensation bin 4, further reducing the difficulty in treating the wastewater, opening the collection port valve 221, allowing the cyanogen chloride gas generated by the reaction to enter the collection tube 222, and then the mixture enters an aggregate loop 223 for liquefaction, and the liquefied cyanogen chloride enters a second material receiving port 71 from a loop outlet 2232 and is collected to obtain cyanogen chloride.
The foregoing is merely exemplary and illustrative of the principles of the present invention and various modifications, additions and substitutions of the specific embodiments described herein may be made by those skilled in the art without departing from the principles of the present invention or exceeding the scope of the claims set forth herein.

Claims (3)

1. A cyanogen chloride preparation process for cyanate ester resin synthesis is characterized by comprising the following steps: the method comprises the following steps:
step S1: weighing the following raw materials in parts by weight: 10-15 parts of sodium cyanide solution and 7-12 parts of liquid chlorine;
step S2: adding 30 mass percent sodium cyanide solution and water into a stirring kettle, and stirring for 5-10min at the rotation speed of 800-;
step S3: adding the sodium cyanide aqueous solution with the mass fraction of 15% and the liquid chlorine prepared in the step S2 into a reactor, and reacting for 5-10min under the conditions that the temperature is 30-50 ℃ and the pH value is 3-4.5 to prepare cyanogen chloride;
the reactor of step S3, including a base (1), the upper surface of the base (1) is provided with a reaction bin (2), the bottom of the reaction bin (2) is provided with a discharge port (21), the top of the reaction bin (2) is provided with a material collecting port (22), two sides of the discharge port (21) are fixed with a first catheter (23) and a second catheter (24), the top of the material collecting port (22) is fixed with a material collecting pipe (222), the material collecting pipe (222) is communicated with the inside of the material collecting port (22), the end of the material collecting pipe (222) is provided with a material collecting ring pipe (223), the first catheter (23) is communicated with the inside of the second catheter (24), the upper surface of the base (1) is also fixed with a first storage bin (3), a condensation bin (4), a first storage bin (5), a second storage bin (6) and a second storage bin (7), the top of the first storage bin (3) is provided with a first feed port (31), a vertical infusion pipe (32) is arranged inside the first storage bin (3), the top end of the vertical infusion pipe (32) penetrates through the first storage bin (3), the vertical infusion pipe (32) is fixedly connected with the first storage bin (3), a booster pump (33) is fixed on the vertical infusion pipe (32), the booster pump (33) is matched with the vertical infusion pipe (32), a liquid spraying pipe (34) is vertically fixed at the top end of the vertical infusion pipe (32), the liquid spraying pipe (34) is communicated with the inside of the vertical infusion pipe (32), a plurality of rows of liquid spraying heads (341) which are uniformly distributed are fixed on the liquid spraying pipe (34), a condensation folding pipe (41) is arranged inside the condensation bin (4), a folding pipe inlet (411) is arranged at one end of the condensation folding pipe (41), a folding pipe outlet (412) is arranged at the other end of the condensation folding pipe (41), the folding pipe inlet (411) and the folding pipe outlet (412) are positioned outside the condensation bin (4), a water inlet (42) is arranged at the bottom end of one side of the condensation bin (4), a water outlet (43) is arranged at one end of the upper surface of the condensation bin (4) far away from the water inlet (42), a pipe folding inlet (411) is communicated with a second liquid guide pipe (24), a first material receiving opening (51) is arranged at one side of the first material receiving bin (5), the first material receiving opening (51) is matched with a pipe folding outlet (412), a heater (61) is fixed on the side wall of the second storage bin (6), a first air guide pipe (62) is fixed at the top end of the second storage bin (6), the first air guide pipe (62) is communicated with the inside of the second storage bin (6), a second air guide pipe (63) is vertically fixed at the top end of the first air guide pipe (62), the second air guide pipe (63) is communicated with the inside of the first air guide pipe (62), third air guide pipes (64) are fixed at the upper side and the lower side of the end of the second air guide pipe (63), the third air guide pipes (64) are communicated with the inside of the second air guide pipe (63), and an air injection pipe (65) is fixed at the end of the third air guide pipe (64), the gas injection pipe (65) is positioned inside the reaction bin (2), the second storage bin (6) is provided with a second feeding hole (67), the top end of the second material receiving groove (7) is provided with a second material receiving hole (71), and the second material receiving hole (71) is matched with the material collecting ring pipe (223);
four supporting columns (25) which are uniformly distributed are fixed between the reaction bin (2) and the base (1), a discharge port valve (211) is arranged inside the discharge port (21), a collection port valve (221) is arranged inside the collection port (22), a first liquid guide valve (231) is arranged inside one end, close to the discharge port (21), of the first liquid guide pipe (23), and a second liquid guide valve (241) is arranged inside one end, close to the discharge port (21), of the second liquid guide pipe (24);
the top end of the collecting ring pipe (223) is provided with a ring pipe inlet (2231), the bottom end of the collecting ring pipe (223) is provided with a ring pipe outlet (2232), the ring pipe inlet (2231) is communicated with the material collecting pipe (222), and the ring pipe outlet (2232) is communicated with the second material receiving port (71);
the end of the first material receiving port (51) is provided with threads, the end of the first material receiving port (51) is connected with a connector (52) in a threaded mode, the end of the pipe folding outlet (412) is provided with threads, and the pipe folding outlet (412) is connected with the connector (52) in a threaded mode;
the jet-propelled pipe (65) on be fixed with a plurality of jet-propelled side pipe (66) that set up relatively, open a plurality of evenly distributed's air jet (661) on jet-propelled side pipe (66), jet-propelled pipe (65) are mutually perpendicular with hydrojet pipe (34), both sides about jet-propelled pipe (65) are located hydrojet pipe (34), be equipped with air-blower (631) on second air duct (63).
2. The process for preparing cyanogen chloride for cyanate ester resin synthesis according to claim 1, wherein: the liquid spraying heads (341) are positioned in the reaction bin (2), the number of each row of liquid spraying heads (341) is four, each row of liquid spraying heads (341) are arranged in a cross shape, the liquid spraying pipe (34) is positioned at the center of the inner part of the reaction bin (2), the liquid spraying pipe (34) is fixedly connected with the reaction bin (2), and the liquid spraying pipe (34) and the liquid spraying heads (341) are made of polytetrafluoroethylene.
3. The process for preparing cyanogen chloride for cyanate ester resin synthesis according to claim 1, wherein: the specific operation steps of step S3 are as follows:
adding a sodium cyanide aqueous solution into a first storage bin (3) from a first feeding hole (31), adding liquid chlorine into a second storage bin (6) from a second feeding hole (67), starting a heater (61) to heat the liquid chlorine, enabling chlorine to enter a second air guide pipe (63) from a first air guide pipe (62), starting an air blower (631) and a booster pump (33), pressing the sodium cyanide aqueous solution in the first storage bin (3) into a liquid spraying pipe (34) from a liquid conveying vertical pipe (32) by the booster pump (33), spraying out the sodium cyanide aqueous solution from a liquid spraying head (341), driving the chlorine to enter a third air guide pipe (64) by the air blower (631), further entering an air spraying pipe (65), dispersing the chlorine into an air spraying side pipe (66), spraying out from an air spraying port (661), enabling the chlorine to be fully contacted with the sodium cyanide aqueous solution when the chlorine enters a reactor due to the air spraying pipes (65) being positioned at the upper side and the lower side of the liquid spraying pipe (34), and enabling the chlorine to be fully contacted with the sodium cyanide aqueous solution at the temperature of 30-50 ℃, the reaction is carried out for 5-10min under the condition that the pH value is 3-4.5, atomized sodium cyanide water solution is gathered at the bottom of a reaction bin (2), a discharge port valve (211) and a first liquid guide valve (231) are opened, the sodium cyanide water solution enters a first storage bin (3) again, so that unreacted sodium cyanide water solution enters the reaction bin (2) again, after the reaction is finished, the first liquid guide valve (231) is closed, a second liquid guide valve (241) is opened, water is introduced from a water inlet (42) and discharged from a water outlet (43), waste water generated by the reaction enters a condensation folding pipe (41) from a folding pipe inlet (411) for cooling, the cooled waste water enters a first receiving bin (5) from a folding pipe outlet (412), a material collecting port valve (221) is opened, cyanogen chloride gas generated by the reaction enters a material collecting pipe (222) and then enters an aggregate ring pipe (223) for liquefaction, and the liquefied cyanogen chloride enters a second material receiving port (71) from a loop pipe outlet (2232) and is collected to obtain the cyanogen chloride.
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CN115025604A (en) * 2021-03-05 2022-09-09 江苏国威化工有限公司 Dechlorination device and process in chlorinated paraffin production process
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3109831A (en) * 1960-11-14 1963-11-05 Pittsburgh Plate Glass Co Cooking polyesters of polybasic acids and polyhydric alcohols in the absence of solvents
CN103071444A (en) * 2013-01-30 2013-05-01 北京工商大学 Gas-liquid reaction device
CN106492731A (en) * 2016-12-23 2017-03-15 马鞍山科英合成材料有限公司 A kind of production equipment for preparing blocked isocyanate
CN110902696A (en) * 2019-08-28 2020-03-24 扬州天启新材料股份有限公司 Preparation method of cyanogen chloride

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3109831A (en) * 1960-11-14 1963-11-05 Pittsburgh Plate Glass Co Cooking polyesters of polybasic acids and polyhydric alcohols in the absence of solvents
CN103071444A (en) * 2013-01-30 2013-05-01 北京工商大学 Gas-liquid reaction device
CN106492731A (en) * 2016-12-23 2017-03-15 马鞍山科英合成材料有限公司 A kind of production equipment for preparing blocked isocyanate
CN110902696A (en) * 2019-08-28 2020-03-24 扬州天启新材料股份有限公司 Preparation method of cyanogen chloride

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
Influence of Reactor and Condensation System Design on Type Pyrolysis Products Yields;Mkhize N M et al.;《Journal of Analytical and Applied Pyrolysis》;20191031;第143卷;第1-8页 *
三聚氯氰的生产和工艺改进;抚顺市染料化工广;《辽宁化工》;19770630;第17-19页 *
氯化氰的应用及生产工艺研究;郗凌霄等;《精细与专用化学品》;20170930(第9期);第6-8页 *

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