Process for efficiently recovering camphor residues
By using a highly efficient dissolving solvent mixed with co-solvent solvent and copper treatment reagent, the problem of difficulty in recycling camphor residue is solved, and efficient recycling and reuse of camphor residue is achieved, reducing environmental pollution and improving resource utilization.
Patent Information
- Application Number
- CN202411501468.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-10-25
- Publication Date
- 2025-02-14
AI Technical Summary
The prior art is difficult to efficiently recycle and reuse camphor residues generated during industrial synthesis of camphor, resulting in waste of resources and environmental pollution.
Using a highly efficient dissolving solvent made of a mixture of co-solvent solvent and copper treatment reagent, the copper oxide, copper element and basic copper carbonate in the camphor residue are removed by complexation reaction, and the camphor and carbonized polymer oil are fully dissolved. , to achieve classified recycling.
It realizes efficient recycling and reuse of camphor residue, reduces environmental pollution, improves the reuse rate of resources, and has good economic benefits.
Smart Images
Figure CN119431131A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of chemical preparation, and more specifically, to a process for efficiently recovering camphor residues. The invention also discloses a solvent that can efficiently dissolve the camphor residues. Background Art
[0002] Synthetic camphor is also called camphor, with a molecular formula of C 10 H 12 O is a white crystal with a refreshing smell, easily soluble in organic solvents and easy to sublime. Synthetic camphor can be used directly as medicine or as an intermediate for the preparation of medicines, as a raw material for industrial and daily camphor products, and as a fragrance.
[0003] Synthetic camphor in industry is generally based on turpentine as raw material, adopts isomerization method, generates the intermediate of camphene, and finally obtains synthetic camphor finished product.This method needs to use basic copper carbonate as dehydrogenation catalyst when isoborneol is carried out dehydrogenation reaction stage, and basic copper carbonate mainly exists in the form of copper element and copper oxide after dehydrogenation reaction ends, and the solvent after dehydrogenation reaction finally obtains finished product camphor through vaporization and sublimation process.In isoborneol dehydrogenation process, along with the increase of reaction number, a certain amount of camphor residues can be accumulated at the bottom of reactor, and there are camphor (about 30%), copper oxide, copper element, basic copper carbonate, carbonized polymer oil and lime in the components of camphor residues, and these camphor residues can reduce the conversion rate of dehydrogenation reaction and the quality of camphor, and it is necessary to regularly discharge the camphor residues at the bottom of reactor.The camphor residues discharged are very viscous liquid after cooling, and these camphor residues are directly treated as hazardous waste products at present, which not only causes pollution, but also wastes resources, and has poor economic benefits. Therefore, it is urgent to design a method that can reasonably recycle camphor residues to solve the above problems. Summary of the invention
[0004] The invention aims to provide a solvent for efficiently dissolving camphor residues. The solvent can be used to remove copper oxide, copper element and basic copper carbonate in the camphor residues by complexation and precipitation, and camphor and carbonized polymer oil can be fully dissolved so as to classify and recycle these substances. The solvent has the characteristics of less pollution, high reuse rate and good economic benefit.
[0005] Another object of the present invention is to provide a process for efficiently recovering camphor residues by utilizing the solvent.
[0006] The first technical solution adopted by the present invention is as follows:
[0007] A solvent for efficiently dissolving camphor residue is prepared by mixing a co-solvent and a copper treatment agent, wherein the co-solvent comprises xylene and a combined solvent, wherein the combined solvent comprises one or more of ethyl acetate, ethanol, acetic acid, and α-pinene alcohol, and the copper treatment agent comprises oxalic acid and a second copper treatment agent, wherein the second copper treatment agent comprises one or more of chromic acid, carbonic acid, and sodium oxalate.
[0008] Furthermore, the weight ratio of the co-solvent and the copper treatment reagent is 90-99 parts: 1-10 parts, the weight ratio of xylene to the combined solvent in the co-solvent is 50-70 parts: 30-50 parts, and the weight ratio of oxalic acid to the second copper treatment agent in the copper treatment reagent is 10-60 parts: 40-90 parts.
[0009] Furthermore, the weight ratio of the co-solvent and the copper treatment reagent is 95 parts:5 parts, the weight ratio of xylene to the combined solvent in the co-solvent is 60 parts:40 parts, and the weight ratio of oxalic acid to the second copper treatment agent in the copper treatment reagent is 40 parts:60 parts.
[0010] Another technical solution adopted by the present invention is as follows:
[0011] A process for efficiently recovering camphor residues comprises the following steps:
[0012] S1, respectively preparing a co-solvent and a copper treatment reagent in proportion and mixing them to obtain a solvent for efficiently dissolving camphor residue;
[0013] S2, putting the solvent for efficiently dissolving camphor residue obtained in step S1 into a dissolving pot in proportion with the camphor residue, heating and stirring until completely dissolved, standing and settling, and then filtering to obtain a precipitate and a filtrate;
[0014] S3, the precipitate obtained in step S2 is subjected to copper recovery treatment, the filtrate is sent to a camphor residue recovery pot for water vapor distillation, steam is transported to a hydrocondensate collection box to obtain hydrocondensate, and the hydrocondensate is sent to a solvent distillation tower for rectification treatment.
[0015] S4, the crude camphor liquid after water vapor distillation in the camphor residue recovery pot is sent to the dehydrogenation pot for drip distillation, and after the brain oil is distilled out, the crude camphor in the pot is sublimated to obtain finished camphor.
[0016] Furthermore, the method further comprises step S5, wherein the various solvents obtained after the distillation treatment in the distillation tower in step S3 are sent to a solvent storage tank, the kettle liquid of the distillation tower is sent to a crystallization box for crystallization and then centrifuged to obtain crude camphor, and the crude camphor is sent to a dehydrogenation pot for sublimation to obtain finished camphor.
[0017] Furthermore, the method further comprises step S6, sending the naphtha distilled in step S4 to a crystallization box, centrifuging to obtain crude camphor after crystallization, and sending the crude camphor to a dehydrogenation pot for sublimation to obtain finished camphor.
[0018] Furthermore, the method further comprises step S7, sending the mother liquor in the crystallization box in steps S5 and S6 to a dehydrogenation kettle for de-heavy distillation, sending the distillate to a crystallization box, centrifuging after crystallization to obtain crude camphor, and sending it to a dehydrogenation pot for sublimation to obtain finished camphor.
[0019] Furthermore, the remaining kettle liquid in the dehydrogenation pot after sublimation in steps S4, S5, S6 and S7 is sent to the residual oil tank and then barreled.
[0020] Furthermore, in step S2, the temperature of the solvent in the dissolving pot is controlled at 60° C., and the stirring time is 1 hour.
[0021] Compared with the prior art, the present invention has the following beneficial effects:
[0022] 1. A solvent for efficiently dissolving camphor residue of the present invention is formed by mixing a co-solvent and a copper treatment reagent, wherein the copper treatment reagent can carry out a complex reaction on copper oxide, copper element and basic copper carbonate in the camphor residue, and then remove the resulting sediment, so as to remove the copper oxide, copper element and basic copper carbonate in the camphor residue;
[0023] The camphor and carbonized polymer oil in the camphor residue can be fully dissolved by the co-dissolving solvent, so as to classify and recycle these substances, reduce the pollution of the camphor residue to the environment, improve its reuse rate, and have good economic benefits;
[0024] The co-solvent includes xylene and a combined solvent, and the combined solvent includes one or more of ethyl acetate, ethanol, acetic acid, and α-pinene alcohol, which can improve the dissolution rate of the co-solvent to the camphor residue, accelerate the dissolution speed, and the water vapor distillation product has a higher purity;
[0025] The copper treatment reagent includes oxalic acid and a second copper treatment agent, and the second copper treatment agent includes one or more of chromic acid, carbonic acid, and sodium oxalate. The combination of at least two compounds can make the complexation reaction of copper materials in camphor residue more complete.
[0026] The solvent can be used to remove copper oxide, copper element and basic copper carbonate in camphor residue by complexation and precipitation, and camphor and carbonized polymer oil can be fully dissolved.
[0027] 2. A process for efficiently recovering camphor residues of the present invention comprises the following steps: firstly preparing a solvent for efficiently dissolving camphor residues in proportion, putting the solvent and the camphor residues into a dissolving pot in proportion to fully dissolve and react, recovering copper from the filtered precipitate, distilling the filtrate to recover various solvents, and then performing a drip distillation on the crude camphor liquid in the dehydrogenation pot. After the naphtha is distilled out, the crude camphor in the dehydrogenation pot is sublimated to obtain a finished camphor product. Such a recovery process can fully recover and reuse the camphor residues, thereby preventing the camphor residues from polluting the environment and improving the reuse rate. BRIEF DESCRIPTION OF THE DRAWINGS
[0028] The drawings described herein are used to provide a further understanding of the present invention and constitute a part of this application. The exemplary embodiments of the present invention and their descriptions are used to explain the present invention and do not constitute an improper limitation of the present invention. In the drawings:
[0029] Figure 1 The present invention is a schematic diagram of the preparation process of the process for efficiently recovering camphor residues. DETAILED DESCRIPTION
[0030] The technical solution of the present invention is further described in detail below in conjunction with specific implementation methods, but does not constitute any limitation to the present invention.
[0031] The invention discloses a solvent for efficiently dissolving camphor residues, which is formed by mixing a co-solvent and a copper treatment agent, wherein the co-solvent comprises xylene and a combined solvent, wherein the combined solvent comprises one or more of ethyl acetate, ethanol, acetic acid, and α-pinene alcohol, so that the dissolution rate of the co-solvent on the camphor residues can be improved, the dissolution speed can be accelerated, and the purity of the water vapor distillation product is higher. The copper treatment agent comprises oxalic acid and a second copper treatment agent, wherein the second copper treatment agent comprises one or more of chromic acid, carbonic acid, and sodium oxalate, and the copper treatment agent comprises a combination of at least two compounds, so that the complexation reaction of copper materials in the camphor residues can be more sufficient.
[0032] The invention discloses a solvent for efficiently dissolving camphor residues. The copper oxide, copper element and basic copper carbonate in the camphor residues can be subjected to complex reaction by using a copper treatment reagent, and then the precipitates are removed, so as to remove the copper oxide, copper element and basic copper carbonate in the camphor residues. The co-solvent can fully dissolve the camphor and carbonized polymer oil in the camphor residues, so as to classify and recycle these substances, reduce the pollution of the camphor residues to the environment, improve the reuse rate thereof, and achieve good economic benefits.
[0033] Furthermore, the weight ratio of the co-solvent and the copper treatment reagent is 90-99 parts: 1-10 parts, the weight ratio of xylene to the combined solvent in the co-solvent is 50-70 parts: 30-50 parts, and the weight ratio of oxalic acid to the second copper treatment agent in the copper treatment reagent is 10-60 parts: 40-90 parts. By reasonably matching the co-solvent and the copper treatment reagent, and combining the reasonable matching ratios of various substances in the co-solvent and the copper treatment reagent, the complexing reaction effect of the solvent can be improved, the reaction can be more complete, and the recovery and reuse rate of camphor residue can be improved.
[0034] Furthermore, the weight ratio of the co-solvent and the copper treatment reagent is 95 parts:5 parts, the weight ratio of xylene to the combined solvent in the co-solvent is 60 parts:40 parts, and the weight ratio of oxalic acid to the second copper treatment agent in the copper treatment reagent is 40 parts:60 parts. By combining the co-solvent and the copper treatment reagent and the various substances in the co-solvent and the copper treatment reagent in this ratio, the solvent can achieve the best complexation reaction effect and the reaction is more complete.
[0035] A process for efficiently recovering camphor residues of the present invention comprises the following steps:
[0036] S1. Prepare a co-dissolving solvent and a copper treatment reagent respectively according to a certain proportion and then mix them to obtain a solvent capable of efficiently dissolving camphor residue.
[0037] S2, putting the solvent for efficiently dissolving camphor residue obtained in step S1 into a dissolving pot in proportion with the camphor residue, heating and stirring until completely dissolved, standing and settling, and then filtering to obtain a precipitate and a filtrate.
[0038] Furthermore, in the step S2, the temperature of the solvent in the dissolving pot is controlled at 60° C. and the stirring time is 1 hour, so that the camphor residue is completely dissolved in the solvent and the copper material in the camphor residue is fully reacted with the copper treatment reagent.
[0039] S3, the precipitate obtained in step S2 is subjected to copper recovery treatment, the filtrate is sent to a camphor residue recovery pot for water vapor distillation, steam is transported to a hydrocondensate collection box to obtain hydrocondensate, and the hydrocondensate is sent to a solvent distillation tower for rectification treatment.
[0040] S4, the crude camphor liquid after water vapor distillation in the camphor residue recovery pot is sent to the dehydrogenation pot for drip distillation, and after the brain oil is distilled out, the crude camphor in the pot is sublimated to obtain finished camphor.
[0041] Furthermore, the method further comprises step S5, wherein the various solvents obtained after the distillation treatment in the distillation tower in step S3 are sent to a solvent storage tank, the kettle liquid of the distillation tower is sent to a crystallization box for crystallization and then centrifuged to obtain crude camphor, and the crude camphor is sent to a dehydrogenation pot for sublimation to obtain finished camphor.
[0042] Furthermore, the method further comprises step S6, sending the naphtha distilled in step S4 to a crystallization box, centrifuging to obtain crude camphor after crystallization, and sending the crude camphor to a dehydrogenation pot for sublimation to obtain finished camphor.
[0043] Furthermore, the method further comprises step S7, sending the mother liquor in the crystallization box in steps S5 and S6 to a dehydrogenation kettle for de-heavy distillation, sending the distillate to a crystallization box, centrifuging after crystallization to obtain crude camphor, and sending it to a dehydrogenation pot for sublimation to obtain finished camphor.
[0044] Furthermore, it is characterized in that the remaining kettle liquid in the dehydrogenation pot after sublimation in steps S4, S5, S6 and S7 is sent to the residual oil tank and then barreled.
[0045] The process for efficiently recovering camphor residues of the present invention can fully recover and reuse the camphor residues, thereby preventing the camphor residues from polluting the environment and improving the reuse rate of the camphor residues.
[0046] The above description is only a preferred embodiment of the present invention. Any modifications, equivalent substitutions and improvements made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims
1. A solvent for efficiently dissolving camphor residues, characterized in that: The invention is formed by mixing a co-solvent and a copper treatment agent, wherein the co-solvent includes xylene and a combined solvent, wherein the combined solvent includes one or more of ethyl acetate, ethanol, acetic acid, and α-pinene alcohol, and the copper treatment agent includes oxalic acid and a second copper treatment agent, wherein the second copper treatment agent includes one or more of chromic acid, carbonic acid, and sodium oxalate.
2. A solvent for efficiently dissolving camphor residue according to claim 1, characterized in that: The weight ratio of the co-solvent and the copper treatment reagent is 90-99 parts:1-10 parts, the weight ratio of xylene to the combined solvent in the co-solvent is 50-70 parts:30-50 parts, and the weight ratio of oxalic acid to the second copper treatment agent in the copper treatment reagent is 10-60 parts:40-90 parts.
3. A solvent for efficiently dissolving camphor residue according to claim 1, characterized in that: The weight ratio of the co-solvent and the copper treatment reagent is 95 parts:5 parts, the weight ratio of xylene to the combined solvent in the co-solvent is 60 parts:40 parts, and the weight ratio of oxalic acid to the second copper treatment agent in the copper treatment reagent is 40 parts:60 parts.
4. A process for efficiently recovering camphor residues, characterized in that: The following steps are involved: S1, respectively preparing a co-dissolving solvent and a copper treatment reagent in proportion and mixing them to obtain a solvent for efficiently dissolving camphor residue as claimed in claim 1; S2, putting the solvent for efficiently dissolving camphor residue obtained in step S1 into a dissolving pot in proportion with the camphor residue, heating and stirring until completely dissolved, standing and settling, and then filtering to obtain a precipitate and a filtrate; S3, the precipitate obtained in step S2 is subjected to copper recovery treatment, the filtrate is sent to a camphor residue recovery pot for water vapor distillation, steam is transported to a hydrocondensate collection box to obtain hydrocondensate, and the hydrocondensate is sent to a solvent distillation tower for rectification treatment. S4, the crude camphor liquid after water vapor distillation in the camphor residue recovery pot is sent to the dehydrogenation pot for drip distillation, and after the brain oil is distilled out, the crude camphor in the pot is sublimated to obtain the finished camphor.
5. A process for efficiently recovering camphor residue according to claim 4, characterized in that: The method further comprises step S5, wherein the various solvents obtained after the distillation treatment in the distillation tower in step S3 are sent to a solvent storage tank, the kettle liquid of the distillation tower is sent to a crystallization box for crystallization, and then centrifuged to obtain crude camphor, and then sent to a dehydrogenation pot for sublimation to obtain finished camphor.
6. A process for efficiently recovering camphor residue according to claim 5, characterized in that: The method further comprises step S6, sending the naphtha distilled in step S4 to a crystallization box, centrifuging to obtain crude camphor after crystallization, and sending the crude camphor to a dehydrogenation pot for sublimation to obtain finished camphor.
7. A process for efficiently recovering camphor residue according to claim 6, characterized in that: The method further comprises step S7, sending the mother liquor in the crystallization box in steps S5 and S6 to a dehydrogenation kettle for de-heavy distillation, sending the distillate to a crystallization box, centrifuging to obtain crude camphor after crystallization, and sending the crude camphor to a dehydrogenation pot for sublimation to obtain finished camphor.
8. A process for efficiently recovering camphor residue according to claim 7, characterized in that: The remaining kettle liquid in the dehydrogenation pot after sublimation in steps S4, S5, S6 and S7 is sent to the residual oil tank and then barreled.
9. A process for efficiently recovering camphor residue according to claim 4, characterized in that: In the step S2, the temperature of the solvent in the dissolving pot is controlled at 60° C. and the stirring time is 1 hour.