CN117105849A - Process for recycling pyridine or pyridine derivative in hexachlorocyclo-triphosphazene synthetic waste residues - Google Patents

Process for recycling pyridine or pyridine derivative in hexachlorocyclo-triphosphazene synthetic waste residues Download PDF

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Publication number
CN117105849A
CN117105849A CN202311023138.9A CN202311023138A CN117105849A CN 117105849 A CN117105849 A CN 117105849A CN 202311023138 A CN202311023138 A CN 202311023138A CN 117105849 A CN117105849 A CN 117105849A
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pyridine
phase
extraction
chlorobenzene
hexachlorocyclotriphosphazene
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李旭锋
龙智
王秋伟
牟永川
金译艇
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Zhejiang Wansheng Co ltd
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Zhejiang Wansheng Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D213/00—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members
    • C07D213/02—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
    • C07D213/04—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom
    • C07D213/06—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom containing only hydrogen and carbon atoms in addition to the ring nitrogen atom
    • C07D213/16—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom containing only hydrogen and carbon atoms in addition to the ring nitrogen atom containing only one pyridine ring

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Pyridine Compounds (AREA)

Abstract

The invention discloses a process for recycling pyridine or pyridine derivatives in hexachlorocyclo-triphosphazene synthetic waste residues, which comprises the following steps: mixing the separated waste residue after the synthesis reaction of hexachlorocyclotriphosphazene with water according to the following ratio of 1: stirring and mixing the mixture in a mass ratio of 0.5-2.5 to obtain a mixture, adding alkali into the mixture to perform a neutralization reaction, controlling the reaction temperature to be 0-50 ℃, and regulating the end point pH value to be 6-10 to obtain a neutralization solution; centrifuging or filtering the neutralization solution to obtain filtrate, and extracting the filtrate with chlorobenzene to obtain an extraction phase and a raffinate phase; rectifying the extract phase to obtain chlorobenzene and recovered pyridine or pyridine derivative. The invention can fully utilize sodium chloride generated by system neutralization, does not need to externally introduce salt, realizes salting-out before extraction, directly returns to the application after salting-out water phase extraction, reduces the wastewater production and wastewater recycling energy consumption, can greatly reduce the extraction difficulty of pyridine or pyridine derivatives, reduces the consumption of extractant, and saves the energy consumption of a rectification separation system.

Description

Process for recycling pyridine or pyridine derivative in hexachlorocyclo-triphosphazene synthetic waste residues
Technical Field
The invention relates to a process for recycling pyridine or pyridine derivatives in hexachlorocyclo triphosphazene synthetic waste residues, and belongs to the technical field of chemical production.
Background
Hexachlorocyclotriphosphazene is a very important intermediate, and since two substitutable chlorine atoms are contained on a phosphorus atom, various derivatives can be generated and used as a flame retardant, an adsorbent, an antioxidant and the like.
Hexachlorocyclotriphosphazene is generally prepared by reacting ammonium chloride and phosphorus pentachloride in an inert solvent with metal chlorides such as aluminum chloride, ferric chloride, barium chloride, magnesium chloride, cobalt chloride, manganese chloride, copper chloride, nickel chloride, zinc chloride, calcium chloride and the like as catalysts, pyridine or pyridine derivatives (C1-C3 alkoxypyridine) and the like as acid binding agents at a certain temperature, generating pyridine hydrochloride which is insoluble in the inert solvent after the reaction is completed, mixing the pyridine hydrochloride with the metal chlorides and excessive ammonium chloride to form solid, separating the solid and the liquid, and disposing the solid and the liquid as waste residues. About 0.6 to 0.8 ton of waste residue is produced by each 1 ton of hexachlorocyclotriphosphazene, the waste residue mainly contains pyridine hydrochloride (or pyridine derivative hydrochloride), ammonium chloride, metal chloride serving as a catalyst and a small amount of solvent, the content of the pyridine hydrochloride (or pyridine derivative hydrochloride) is 50 to 70 percent, the content of the ammonium chloride is 10 to 35 percent, the content of the metal chloride is 5 to 20 percent, and the balance is chlorobenzene and other impurities, so that no document or patent report about pyridine recovery in the waste residue is seen at present.
Chinese patent CN201410684338.3 proposes PCl 5 、NH 4 Cl is reacted in chlorobenzene solvent with ferric chloride, zinc chloride and magnesium chloride as composite catalyst and pyridine as acid binding agent to obtain hexachlorocyclotriphosphazene, and the waste residue containing pyridine hydrochloride is filtered and distilled under reduced pressure to obtain hexachlorocyclotriphosphazene crude product. The patent does not mention the way in which the waste residue containing pyridine hydrochloride is disposed.
Chinese patent CN200610116011.1 proposes PCl 5 、NH 4 Cl reacts in chlorobenzene solvent with magnesium chloride, aluminum chloride or zinc chloride as catalyst and pyridine or C1-C3 alkoxyl pyridine as acid-binding agent at reflux temperature to obtain hexachlorocyclotriphosphazene. The patent does not mention the way in which the waste residue containing pyridine hydrochloride is disposed.
Chinese patent CN202211506957.4 proposes that hexachlorocyclotriphosphazene is prepared by heating reaction with ionic liquid (prepared by mixing chlorobenzene, composite metal chloride and pyridine and then introducing HCl) as catalyst in chlorobenzene solvent with phosphorus pentachloride chlorobenzene solution and ammonium chloride, filtering to remove waste residue, and recovering chlorobenzene by vacuum distillation. The patent does not mention the way in which the waste residue containing pyridine hydrochloride is disposed.
For pyridine recovery, chinese patent CN116023325a proposes mixing aqueous pyridine with benzene, separating pyridine from water by azeotropic distillation with benzene carrying water, distilling crude pyridine dehydrated at the bottom of the column to remove heavy components, and recycling. The method can obtain low-water-content pyridine, but is only suitable for high-concentration water-content pyridine, and has the problems of large benzene consumption and high energy consumption for the low-concentration water-content pyridine. The method has poor applicability to pyridine recovery in hexachlorocyclotriphosphazene.
Chinese patent CN107474010B proposes a process of twice salting-out extraction of aqueous pyridine with addition of sodium chloride and potassium carbonate to saturation. The method has the advantages of general dewatering effect and low pyridine recovery rate.
Chinese patent CN101074211B proposes a process for recovering pyridine by vacuum distillation after extracting aqueous pyridine with biodiesel containing fatty acid methyl ester, which has very low water solubility. The method has the advantages that although the used extractant and pyridine are easy to separate due to large boiling point difference, the single extraction rate is low, the using amount of the extractant is large, and the total extraction rate can be ensured only by more times of extraction.
Chinese patent CN201210581379.0 proposes that pyridine hydrochloride is neutralized with alkali at 55-60 deg.c, and then twice mixed distilled with dichloroethane, and the fraction is separated and layered through standing, and the recovered pyridine is obtained through rectifying the organic phase with recovery rate up to 90-95%. The method can obtain the recovered pyridine with higher purity, and has higher recovery rate, but complicated operation and high energy consumption.
Disclosure of Invention
Aiming at the technical problems in the prior art, the invention aims to provide a process for recycling pyridine or pyridine derivatives in hexachlorocyclotriphosphazene synthetic waste residues.
In order to achieve the above purpose, the present invention provides the following technical solutions:
a process for recovering pyridine or pyridine derivatives in hexachlorocyclotriphosphazene synthetic waste residues comprises the following steps:
1) Mixing the separated waste residue and water after the synthesis reaction of hexachlorocyclotriphosphazene to obtain a mixture, wherein the mass ratio of the waste residue to the water is 1:0.5 to 2.5.
2) Adding alkali into the mixture in the step 1) to perform neutralization reaction, controlling the reaction temperature to be 0-50 ℃, and regulating the pH value of the end point to be 6-10 to obtain a neutralization solution. The alkali is solid sodium hydroxide, sodium hydroxide solution, solid sodium carbonate, sodium carbonate solution, solid sodium bicarbonate, sodium bicarbonate solution or a mixture thereof.
3) And (3) centrifuging or filtering the neutralization solution obtained in the step (2) to obtain filtrate, and extracting the filtrate with chlorobenzene to obtain an extraction phase and a raffinate phase.
4) Rectifying the extract phase in the step 3) to obtain chlorobenzene and recovered pyridine or pyridine derivatives.
The process step 1) is further characterized in that the mass ratio of waste residues to water is preferably 1:0.5-1.6.
The above process step 2), further, the reaction temperature is preferably from room temperature to 40 ℃, preferably the end point pH is adjusted to 6-8.
Still further, standing the filtrate obtained in the step 3) for phase separation to obtain a water phase and a salt phase, and extracting the salt phase and the water phase with chlorobenzene to obtain an extraction phase, a salt phase raffinate phase and a water phase raffinate phase.
Still further, the aqueous phase raffinate phase is applied to the step 1) and is used for being stirred and mixed with waste residues to prepare a mixture.
Still further, the salt phase raffinate phase adopts azeotropic distillation to distill azeotropic components containing residual pyridine, and the azeotropic components are applied to the step 3) for extraction by chlorobenzene.
The process step 3) further comprises the steps of intermittent extraction or countercurrent continuous extraction, wherein the intermittent extraction times are 1-5 times.
Further, the dosage of chlorobenzene as an extractant for each batch extraction is 0.3-2 times of the mass of water in the neutralization solution.
Further, the countercurrent continuous extraction is carried out, and the ratio of the mass flow of the extractant to the mass flow of the neutralization liquid is 0.3-1.8: 1.
and 4) further, carrying out azeotropic distillation dehydration, molecular sieve dehydration or pervaporation membrane dehydration on the extract phase to obtain a dehydrated extract phase, rectifying the dehydrated extract phase, obtaining recovered pyridine or pyridine derivatives from the top of the tower, and applying the residual tower bottom liquid to the step 3) as an extractant.
The process step 4) further comprises the step of recycling the recovered pyridine or pyridine derivative as an acid binding agent or catalyst to use chlorobenzene as a solvent and PCl 5 And NH 4 Cl is used as a raw material in the reaction for preparing hexachlorocyclotriphosphazene.
Still further, the pyridine or pyridine derivative used in the sleeve is allowed to contain more chlorobenzene, and the chlorobenzene content is less than or equal to 90%.
Compared with the prior art, the invention has the following beneficial effects:
1) The invention has high pyridine recovery rate, the recovery rate of high-value pyridine or pyridine derivatives in waste residue can reach more than 95-99%, the pyridine consumption for synthesizing hexachlorocyclotriphosphazene is greatly reduced, and the cost is saved.
2) The pyridine recovered by the method can be directly reused in the hexachlorocyclotriphosphazene synthesis process under the condition of containing more chlorobenzene, does not influence the hexachlorocyclotriphosphazene synthesis effect, greatly reduces the rectification difficulty of pyridine recovery, and saves energy consumption. Meanwhile, the pretreatment of removing the residual solvent chlorobenzene from the initial waste residue is not needed before recycling, and the recycling of the residual chlorobenzene can be realized, so that the equipment investment, the material consumption and the energy consumption are saved.
3) The invention can fully utilize sodium chloride generated by system neutralization, does not need to externally introduce salt, realizes salting out before extraction, directly returns to the application after salting out water phase extraction, reduces the production amount of wastewater and the energy consumption for wastewater reuse, and can greatly reduce the extraction difficulty, reduce the consumption of extractant and save the energy consumption of a rectification separation system due to low pyridine content of salting out salt phase and high pyridine content but less water content of salting out water phase.
Drawings
FIG. 1 is a block diagram of the process for recovering pyridine or pyridine derivatives from hexachlorocyclotriphosphazene synthetic waste residues according to the present invention.
Detailed Description
The invention will be further illustrated with reference to specific examples, but the scope of the invention is not limited thereto.
Example 1:
the process for recovering pyridine or pyridine derivatives from hexachlorocyclotriphosphazene synthetic waste residues by adopting a flow frame shown in figure 1 comprises the following steps:
1) The waste residue separated after the synthesis reaction of hexachlorocyclotriphosphazene is finished comprises the following components in parts by weight: the pyridine hydrochloride content was 53.65%, ammonium chloride 26.52%, metal chlorides (iron chloride, zinc chloride, magnesium chloride mixture) 15.66%, the balance chlorobenzene solvents and other impurities.
And stirring and mixing the waste residues and water according to the mass ratio of 1:1.2 to obtain a mixture.
2) Slowly adding caustic soda flakes into the mixture obtained in the step 1) to perform neutralization reaction, controlling the reaction temperature to be 25-30 ℃, and regulating the pH value of the end point to be 6-7 to obtain a neutralization solution;
3) Filtering the neutralization solution in the step 2), standing and phase-separating the filtrate to obtain a water phase and a salt phase, extracting the salt phase with extracting agent chlorobenzene, and then extracting the water phase to obtain an extraction phase, a salt phase raffinate phase and a water phase raffinate phase, wherein the water phase raffinate phase is applied to the step 1) and is used for being stirred and mixed with waste residues to prepare a mixture.
Wherein the extraction is carried out in an intermittent extraction mode, the extraction times are 5 times, and the chlorobenzene dosage of each extractant is 0.3 times of the water mass in the neutralization liquid.
4) And 3) distilling the salt phase raffinate phase in the step 3) by adopting azeotropic distillation to obtain azeotropic components containing residual pyridine, wherein the azeotropic components are applied to the step 3) for extraction by chlorobenzene, and the distillation residues are treated as waste brine. In addition, the extraction phase obtained in the step 3) is subjected to molecular sieve dehydration, the dehydrated extraction phase is subjected to rectification, the pyridine recovered from the top of the tower contains more chlorobenzene, the chlorobenzene content is 55.73%, and the residual tower bottom liquid is used as an extractant in the step 3).
When the production method is stably operated, the obtained pyridine basically contains two components of pyridine and chlorobenzene, the pyridine content is (55-60)% +/-1%, the chlorobenzene content is about 40-45%, the moisture content is lower than 0.05%, and the pyridine recovery rate can be more than 95-99%.
The pyridine obtained by recycling is used as an acid binding agent, chlorobenzene is used as a solvent, a mixture of ferric chloride, zinc chloride and magnesium chloride is used as a catalyst, and PCl 5 And NH 4 In the reaction for preparing hexachlorocyclotriphosphazene by taking Cl as a raw material, the reaction yield of the hexachlorocyclotriphosphazene can reach more than 90 percent, and the experimental effect which is the same as or similar to that of fresh pyridine used as an acid binding agent is basically obtained.
Example 2:
the process for recovering pyridine or pyridine derivatives from hexachlorocyclotriphosphazene synthetic waste residues by adopting a flow frame shown in figure 1 comprises the following steps:
1) The waste residue separated after the synthesis reaction of hexachlorocyclotriphosphazene is finished comprises the following components in parts by weight: the pyridine hydrochloride content was 67.42%, ammonium chloride 14.33%, metal chlorides (cobalt chloride, aluminum chloride, magnesium chloride mixture) 14.27%, the balance chlorobenzene solvents and other impurities.
And (3) stirring and mixing the waste residues and water according to a mass ratio of 1:0.5 to obtain a mixture.
2) Dropwise adding 30% concentration liquid alkali into the mixture in the step 1) to perform neutralization reaction, controlling the reaction temperature to be 45-50 ℃, and regulating the end point pH value to 8-9 to obtain a neutralization solution;
3) Filtering the neutralization solution in the step 2), standing and phase-separating the filtrate to obtain a water phase and a salt phase, extracting the salt phase with extracting agent chlorobenzene, and then extracting the water phase to obtain an extraction phase, a salt phase raffinate phase and a water phase raffinate phase, wherein the water phase raffinate phase is applied to the step 1) and is used for being stirred and mixed with waste residues to prepare a mixture.
Wherein the extraction is carried out in an intermittent extraction mode, the extraction times are 2 times, and the chlorobenzene dosage of each extractant is 1 time of the water quality in the neutralization liquid.
4) And 3) distilling the salt phase raffinate phase in the step 3) by adopting azeotropic distillation to obtain azeotropic components containing residual pyridine, wherein the azeotropic components are applied to the step 3) for extraction by chlorobenzene, and the distillation residues are treated as waste brine. In addition, the extract phase obtained in the step 3) is dehydrated by a pervaporation membrane, the dehydrated extract phase is rectified, the recovered pyridine is obtained from the top of the tower, the pyridine contains more chlorobenzene, the chlorobenzene content is 76.35%, and the residual tower bottom liquid is used as an extractant in the step 3).
When the production method is stably operated, the obtained pyridine basically contains two components of pyridine and chlorobenzene, the pyridine content is (75-80)% +/-1%, the chlorobenzene content is about 20-25%, the moisture content is lower than 0.05%, and the pyridine recovery rate can be more than 95-99%.
The pyridine obtained by recycling is used as an acid binding agent, chlorobenzene is used as a solvent, a mixture of ferric chloride, zinc chloride and magnesium chloride is used as a catalyst, and PCl 5 And NH 4 In the reaction for preparing hexachlorocyclotriphosphazene by taking Cl as a raw material, the reaction yield of the hexachlorocyclotriphosphazene can reach more than 90 percent, and the experimental effect which is the same as or similar to that of fresh pyridine used as an acid binding agent is basically obtained.
Example 3:
the process for recovering pyridine or pyridine derivatives from hexachlorocyclotriphosphazene synthetic waste residues by adopting a flow frame shown in figure 1 comprises the following steps:
1) The waste residue separated after the synthesis reaction of hexachlorocyclotriphosphazene is finished comprises the following components in parts by weight: the pyridine hydrochloride content was 53.65%, ammonium chloride 26.52%, metal chlorides (iron chloride, zinc chloride, magnesium chloride mixture) 15.66%, the balance chlorobenzene solvents and other impurities.
And stirring and mixing the waste residues and water according to the mass ratio of 1:1.5 to obtain a mixture.
2) Slowly adding 30% liquid alkali into the mixture in the step 1) to perform neutralization reaction, controlling the reaction temperature to be 15-20 ℃, and regulating the pH value of the end point to be 9-10 to obtain a neutralization solution;
3) Filtering the neutralization solution in the step 2), and extracting the filtrate by using an extracting agent chlorobenzene to obtain an extraction phase and a raffinate phase.
Wherein the extraction is performed in an intermittent extraction mode, the extraction times are 3 times, and the chlorobenzene dosage of each extractant is 1.5 times of the water mass in the neutralization liquid.
4) And 3) distilling the raffinate phase in the step 3) by adopting azeotropic distillation to obtain azeotropic components containing residual pyridine, wherein the azeotropic components are applied to the step 3) for extraction by chlorobenzene, and the distillation residues are treated as waste brine. In addition, the extraction phase obtained in the step 3) is subjected to molecular sieve dehydration, the dehydrated extraction phase is subjected to rectification, the recovered pyridine is obtained from the top of the tower, the pyridine contains more chlorobenzene, the chlorobenzene content is 89.43%, and the residual tower bottom liquid is used as an extractant in the step 3).
When the production method is stably operated, the obtained pyridine basically contains two components of pyridine and chlorobenzene, the pyridine content is (85-90)% +/-1%, the chlorobenzene content is about 10-15%, the moisture content is lower than 0.05%, and the pyridine recovery rate can be more than 95-99%.
The pyridine obtained by recycling is used as an acid binding agent, chlorobenzene is used as a solvent, a mixture of ferric chloride, zinc chloride and magnesium chloride is used as a catalyst, and PCl 5 And NH 4 In the reaction for preparing hexachlorocyclotriphosphazene by taking Cl as a raw material, the reaction yield of the hexachlorocyclotriphosphazene can reach more than 90 percent, and the experimental effect which is the same as or similar to that of fresh pyridine used as an acid binding agent is basically obtained.
What has been described in this specification is merely an enumeration of possible forms of implementation for the inventive concept and may not be considered limiting of the scope of the present invention to the specific forms set forth in the examples.

Claims (9)

1. A process for recovering pyridine or pyridine derivatives in hexachlorocyclo-triphosphazene synthetic waste residues is characterized by comprising the following steps:
1) Mixing the separated waste residue and water after the synthesis reaction of hexachlorocyclotriphosphazene to obtain a mixture, wherein the mass ratio of the waste residue to the water is 1: 0.5-2.5;
2) Adding alkali into the mixture in the step 1) to perform neutralization reaction, controlling the reaction temperature to be 0-50 ℃, and regulating the pH value of the end point to be 6-10 to obtain a neutralization solution; the alkali is solid sodium hydroxide, sodium hydroxide solution, solid sodium carbonate, sodium carbonate solution, solid sodium bicarbonate, sodium bicarbonate solution or a mixture thereof;
3) Centrifuging or filtering the neutralization solution obtained in the step 2) to obtain filtrate, and extracting the filtrate with chlorobenzene to obtain an extraction phase and a raffinate phase;
4) Rectifying the extract phase in the step 3) to obtain chlorobenzene and recovered pyridine or pyridine derivatives.
2. The process for recycling pyridine or pyridine derivatives in hexachlorocyclotriphosphazene synthetic waste residues according to claim 1, wherein in the step 1), the mass ratio of the waste residues to water is 1:0.5-1.6.
3. The process for recovering pyridine or pyridine derivatives from hexachlorocyclotriphosphazene synthetic waste residue according to claim 1, wherein in the step 2), the neutralization reaction temperature is room temperature to 40 ℃.
4. The process for recovering pyridine or pyridine derivatives from hexachlorocyclotriphosphazene synthetic waste residue according to claim 1, wherein in the step 2), the final pH value is adjusted to 6-8.
5. The process for recovering pyridine or pyridine derivatives from hexachlorocyclotriphosphazene synthetic waste residue according to claim 1, wherein the filtrate is subjected to standing phase separation to obtain an aqueous phase and a salt phase, the salt phase is extracted with chlorobenzene, the aqueous phase is extracted again to obtain an extract phase, a salt phase raffinate phase and an aqueous phase raffinate phase, and the aqueous phase raffinate phase is applied to the step 1) and is used for being stirred and mixed with the waste residue to prepare a mixture.
6. The process for recovering pyridine or pyridine derivatives from hexachlorocyclotriphosphazene synthetic waste residue as claimed in claim 5, wherein the salt phase raffinate phase is subjected to azeotropic distillation treatment, an azeotropic component containing residual pyridine is distilled, the distillation residue is waste brine, and the azeotropic component is applied to step 3) for extraction with chlorobenzene.
7. The process for recovering pyridine or pyridine derivatives from hexachlorocyclotriphosphazene synthetic waste residues according to claim 1, wherein the extraction in the step 3) is intermittent extraction or countercurrent continuous extraction, the intermittent extraction times are 1-5 times, the chlorobenzene dosage of each extractant of the intermittent extraction is 0.3-2 times of the water mass in the neutralization liquid, and the ratio of the mass flow of the extractant of the countercurrent continuous extraction to the mass flow of the neutralization liquid is 0.3-1.8: 1.
8. the process for recovering pyridine or pyridine derivatives from hexachlorocyclotriphosphazene synthetic waste residue according to claim 1, wherein the extraction phase in the step 4) is dehydrated by azeotropic distillation, molecular sieve or pervaporation membrane, the dehydrated extraction phase is rectified, the recovered pyridine or pyridine derivatives are obtained from the top of the tower, and the residual tower bottom liquid is used as the extractant in the step 3).
9. The process for recovering pyridine or pyridine derivatives from hexachlorocyclotriphosphazene synthesis waste residue as claimed in claim 8, wherein the recovered pyridine or pyridine derivatives are allowed to contain more chlorobenzene, wherein the chlorobenzene content is less than or equal to 90%, and the recovered pyridine or pyridine derivatives are used as an acid-binding agent or a catalyst sleeve for use in chlorobenzene-based PCl as a solvent 5 And NH 4 Cl is used as a raw material in the reaction for preparing hexachlorocyclotriphosphazene.
CN202311023138.9A 2023-08-15 2023-08-15 Process for recycling pyridine or pyridine derivative in hexachlorocyclo-triphosphazene synthetic waste residues Pending CN117105849A (en)

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