CN115106365A

CN115106365A - Method and device for recycling degradable medical supplies

Info

Publication number: CN115106365A
Application number: CN202210739768.5A
Authority: CN
Inventors: 吕国玉; 唐游; 罗湘; 罗琳; 刘莉
Original assignee: Sichuan Guona Technology Co ltd
Current assignee: Sichuan Guona Technology Co ltd
Priority date: 2022-06-28
Filing date: 2022-06-28
Publication date: 2022-09-27
Anticipated expiration: 2042-06-28
Also published as: CN115106365B

Abstract

The invention discloses a recovery method and a recovery device of degradable medical supplies, wherein the recovery method comprises the following steps: putting the degradable medical supplies, the solvent and the catalyst into a reaction kettle, and stopping vacuumizing when the kettle is vacuumized to below 2000 pa; heating the reaction kettle to 110-130 ℃, and stirring the materials in the kettle to dissolve the degradable medical supplies to form a homogeneous solution; reacting for 10-120 min after the temperature in the kettle rises to 180-250 ℃ to obtain a monomer; carrying out reduced pressure distillation on materials in the reaction kettle, co-distilling the monomer, the coloring agent and the solvent from the reaction kettle, and carrying out secondary reduced pressure distillation on the obtained mixed liquid to obtain colorless and transparent monomer and solvent; dissolving the distillation residue, distilling under reduced pressure again, washing the distillation solid residue with water, and drying to obtain the coloring agent. The recycling device is used for realizing the recycling method. The monomers and the coloring agent recovered by the recovery method can be repeatedly utilized, so that the resource waste is avoided, and the production cost of medical supplies is reduced.

Description

Method and device for recycling degradable medical supplies

Technical Field

The invention relates to the technical field of medical supplies, in particular to a method and a device for recovering degradable medical supplies.

Background

Many of the clinically used medical supplies are made of degradable materials such as ligation clips, sutures, bone plates, tissue repair materials, and the like. In the production process of the medical supplies, a large amount of waste materials or waste products are produced, and the waste materials and expired products cannot flow out of a factory, so that the medical supplies are regarded as solid wastes to be destroyed or destroyed on the spot, resource waste is caused, and the production cost is high.

Disclosure of Invention

Aiming at the defects of the prior art, the invention provides a recovery method and a recovery device of a degradable medical supply, the recovery method can recover monomers and coloring agents in the degradable medical supply, the recovered monomers and coloring agents can be recycled, a new medical supply is prepared, resources are saved, and the production cost is reduced.

The technical scheme adopted by the invention is as follows:

a method of recycling a degradable medical article comprising the steps of:

step S1, putting the degradable medical supplies, the solvent and the catalyst into a reaction kettle, vacuumizing the kettle, and stopping vacuumizing when the pressure in the kettle is reduced to below 2000 pa;

s2, heating the reaction kettle, and stirring the materials in the kettle at a rotating speed of 50-500 r/min when the temperature in the kettle is raised to 110-130 ℃ so as to dissolve the degradable medical supplies in the solvent to form a homogeneous solution of the polymer and the coloring agent;

step S3, when the temperature in the kettle rises to 180-250 ℃, the reaction time is calculated, the reaction is carried out for 10-120 min, a monomer is obtained, and in the reaction process, the materials in the kettle are subjected to condensation reflux;

step S4, after the reaction is finished, vacuumizing the reaction kettle, carrying out reduced pressure distillation on materials in the reaction kettle, co-distilling the monomer, the coloring agent and the solvent out of the reaction kettle, and condensing to obtain a mixed liquid of the monomer and the coloring agent;

step S5, carrying out secondary reduced pressure distillation on the mixed liquid, wherein the distillation temperature is 50-220 ℃, the distillation speed is 60-100 r/min, the distillation pressure is not more than 200pa, and collecting fractions at corresponding temperatures to respectively obtain colorless and transparent monomers and solvents;

and S6, dissolving the distillation residue in the step S5 by ethyl acetate, filtering, distilling the filtrate under reduced pressure again at the temperature of 30-40 ℃ and under the pressure of less than 200pa, and washing and drying the distillation solid residue to obtain a coloring agent.

In the method for recycling a degradable medical article disclosed in the present application, in step S1, the degradable medical article, the solvent, and the catalyst are, in parts by mass: 100 parts of degradable medical supplies, 20-200 parts of solvent and 0.1-5 parts of catalyst.

In the recycling method of the degradable medical supplies disclosed by the application, the degradable medical supplies are absorbable ligature clips, sutures or other medical products which take polydioxanone and a coloring agent as raw materials.

In the method for recycling the degradable medical supplies, in step S1, the solvent is an aromatic ester compound with a boiling point of 300 to 410 ℃, and the aromatic ester compound and the degradable medical supplies are miscible under a heating condition.

In the recycling method of the degradable medical product disclosed in the present application, in the step S2, the coloring agent is solvent violet 13, solvent violet 9, solvent yellow 93, or other coloring agent with a boiling point higher than 450 ℃.

In the method for recycling degradable medical supplies disclosed in the present application, in step S1, the catalyst is one or more of copper oxide, niobium pentoxide, attapulgite, activated clay or other transition metal oxides, and clay-based catalysts.

Based on the same inventive concept, the invention also discloses a recovery device for realizing the recovery method, and particularly,

the utility model provides a recovery unit of degradable medical supplies for retrieve monomer and coloring agent among the degradable medical supplies, including taking rabbling mechanism, heating mechanism's reation kettle, still include:

the collecting tank is communicated with the reaction kettle through a material pipe; one end of the material pipe is connected with the top of the reaction kettle, and the other end of the material pipe extends towards the upper part of the reaction kettle and then inclines downwards to be connected with the collecting tank;

one end of the return pipe is communicated with the reaction kettle, and the other end of the return pipe is communicated with one end of the material pipe which is inclined downwards and is close to the collecting tank;

the vacuum mechanism is communicated with the collecting tank through a vacuum tube;

the distillation equipment is connected with the collecting tank, and the material in the collecting tank enters the distillation equipment for distillation;

wherein, a condensing pipe is sleeved on the outer side of the pipe wall of the material pipe, which is inclined downwards; after the degradable medical supplies react in the reaction kettle to generate monomers and coloring agents, the degradable medical supplies are subjected to reduced pressure distillation in the reaction kettle under the vacuumizing action of the vacuum mechanism, enter the material pipe, are condensed by the condenser pipe and flow into the collection tank; and carrying out secondary reduced pressure distillation on the materials in the collecting tank by using a distillation device, and respectively recovering the monomer, the solvent and the coloring agent.

In the recovery device of the degradable medical supplies, the vacuum mechanism is provided with a buffer tank, and the buffer tank is communicated with the collection tank through the vacuum tube;

the buffer tank is provided with a vacuum pump port and a sewage discharge pipe;

the vacuum pump port is positioned on the upper side of the buffer tank and is connected with a vacuum pump;

the sewage draining pipe is positioned at the bottom of the buffer tank, and a fourth valve is arranged on the sewage draining pipe;

one end of the vacuum pipe is connected with the top of the collecting tank, and the other end of the vacuum pipe extends into the buffer tank from the top of the buffer tank to the position below the vacuum pump port.

In the recycling device of degradable medical supplies disclosed in the present application, the collection tank includes:

the emptying pipe is arranged at the top of the collecting tank, is communicated with the atmosphere and is provided with an exhaust valve;

the discharge pipe is arranged at the bottom of the collecting tank and is provided with a fifth valve;

the manhole is arranged on the upper side of the tank body of the collecting tank;

and one end of the collecting pipe is connected with the material pipe, and the other end of the collecting pipe extends inwards from the top of the collecting tank to the observation area of the manhole.

In the recycling device of the degradable medical supply disclosed in the present application, the recycling device further comprises a controller; the controller is connected with the heating mechanism, the stirring mechanism and the vacuum mechanism;

the reaction kettle is provided with a temperature sensor and a pressure sensor; and the temperature sensor and the pressure sensor are connected with the controller.

Compared with the prior art, the invention has the beneficial effects that:

(1) the degradable medical supplies are heated and dissolved in the reaction kettle to obtain the degradable materials and the coloring agent, the degradable materials, the coloring agent and the solvent form a homogeneous solution, the degradable materials are subjected to cracking reaction in the reaction kettle under the action of the catalyst to generate monomers, the coloring agent and the solvent are co-distilled out of the reaction kettle through reduced pressure distillation, and a mixed liquid is obtained through condensation and relatively directly cracked, the cracking stirring resistance of a solution phase is small, the mass and heat transfer are more uniform, the influence on the product quality due to the fact that local heating of the direct cracking is uneven can be effectively avoided, meanwhile, the monomers and the solvent form a homogeneous solution and are co-distilled, the monomers are prevented from being solidified and blocking a pipeline after contacting with a pipe wall and being cooled, and the industrial production is more favorably realized; and the molecular chain of the polymer in the solution is fully stretched and moved, which is beneficial to increasing the contact area of the polymer and the catalyst and improving the reaction efficiency.

(2) And performing secondary reduced pressure distillation on the mixed liquid by using a rotary evaporator to respectively obtain a colorless and transparent monomer, a solvent and a coloring agent, thereby realizing the recovery of the degradable medical supplies. The monomer and the coloring agent are recovered by the method, the recovery rate is 75-86%, and the purity of the monomer can reach more than 99%. The recovered monomer and the coloring agent can be repeatedly utilized, the resource waste is avoided, the production cost of medical supplies is reduced, and meanwhile, the separated solvent can also be recycled for homogeneous phase cracking of materials.

Drawings

In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present application, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.

FIG. 1 is a schematic flow diagram of a method for recycling a degradable medical article;

FIG. 2 is a schematic view of an absorbable ligature clip;

FIG. 3 is a schematic view of a mixed liquid distilled under reduced pressure from a reaction vessel;

FIG. 4 is a schematic illustration of recovered monomer;

FIG. 5 is a schematic illustration of recovered solvent;

FIG. 6 is a schematic illustration of recovered stain;

FIG. 7 is a schematic view of a recycling device for degradable medical supplies;

fig. 8 is a schematic structural diagram of a collecting pipe and a manhole.

Reference numerals:

1. a reaction kettle; 11. a stirring mechanism; 12. a heating mechanism; 13. heating a jacket; 14. a heat-insulating layer; 15. a pressure sensor; 16. a temperature sensor; 17. an air inlet pipe; 18. a cooling tube;

2. a collection tank; 21. emptying the pipe; 22. a discharge pipe; 23. a manhole; 24. a collection pipe; 25. an exhaust valve; 26. a fifth valve;

3. a material pipe; 31. a first valve; 32. a condenser tube; 33. a condensed water inlet; 34. a condensed water outlet; 35. a return pipe; 36. a second valve; 37. a third valve;

4. a vacuum mechanism; 41. a buffer tank; 42. a vacuum tube; 43. a vacuum pump port; 44. a blow-off pipe; 45. and a fourth valve.

Detailed Description

In order to make the aforementioned objects, features and advantages of the present application more comprehensible, embodiments accompanying the present application are described in detail below with reference to the accompanying drawings. It is to be understood that the specific embodiments described herein are merely illustrative of the application and are not limiting of the application. It should be further noted that, for the convenience of description, only some of the structures related to the present application are shown in the drawings, not all of the structures. 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 application.

The terms "comprising" and "having," as well as any variations thereof, in this application are intended to cover non-exclusive inclusions. For example, a process, method, system, article, or apparatus that comprises a list of steps or elements is not limited to only those steps or elements listed, but may alternatively include other steps or elements not listed, or inherent to such process, method, article, or apparatus.

Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present application, "a plurality" means two or more unless specifically limited otherwise.

Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.

Reference in the specification to "an embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment can be included in at least one embodiment of the specification. The appearances of the phrase in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments. It is explicitly and implicitly understood by one skilled in the art that the embodiments described herein can be combined with other embodiments.

Referring to fig. 1 to 8, an embodiment of the present application provides a method and a device for recycling a degradable medical product, and mainly aims to solve the problems of resource waste and high production cost caused by waste materials and waste products generated in a production process of the degradable medical product and by the fact that an expired product is taken as solid waste and destroyed on the spot.

The degradable medical supplies are made of degradable materials, such as high molecular poly (p-dioxanone) (PPDO) and the like, which are polymerized by monomers and can generate cracking reaction under certain conditions to generate monomer materials. The medical product is usually added with coloring agents, such as solvent violet 13, solvent violet 9, solvent yellow 93, etc. Waste materials and waste products produced in the production process of the degradable medical supplies and overdue products are taken as solid wastes and are destroyed on the spot, so that resource waste is caused, and the production cost is high.

Referring to fig. 1 to 6, the method for recycling a degradable medical article disclosed in the present application includes the following steps:

and step S1, putting the degradable medical supplies, the solvent and the catalyst into a reaction kettle, vacuumizing the kettle, and stopping vacuumizing when the pressure in the kettle is reduced to below 2000 pa.

And S2, heating the reaction kettle, and stirring the materials in the kettle at a rotating speed of 50-500 r/min when the temperature in the kettle is raised to 110-130 ℃ so as to dissolve the degradable medical supplies in the solvent to form a homogeneous solution of the polymer and the coloring agent. After the reaction kettle is heated, the degradable medical supplies are dissolved, the degradable materials, the coloring agent and the solvent form a homogeneous solution, the mass transfer and heat transfer of the homogeneous solution are more uniform, the influence on the product quality caused by the fact that the local part is heated unevenly can be effectively avoided, meanwhile, the molecular chains in the solution of the polymer are fully unfolded and moved, the contact surface between the polymer and the catalyst can be increased, and the reaction efficiency is improved.

And S3, when the temperature in the kettle rises to 180-250 ℃, calculating the reaction time, reacting for 10-120 min to obtain a monomer, and condensing and refluxing the materials in the kettle in the reaction process. The degradable material is subjected to cracking reaction under the action of a catalyst under the conditions of high temperature and low pressure to generate a monomer.

And step S4, after the reaction is finished, vacuumizing the reactor, carrying out reduced pressure distillation on the materials in the reactor, co-distilling the monomer, the coloring agent and the solvent out of the reactor, and condensing to obtain a mixed liquid of the monomer and the coloring agent. Monomer and solvent form homogeneous phase solution to be co-distilled, which can prevent monomer from contacting pipe wall and cooling to solidify and block pipe, and raise monomer recovering rate.

And step S5, carrying out secondary reduced pressure distillation on the mixed liquid, wherein the distillation temperature is 50-220 ℃, the distillation speed is 60-100 r/min, the distillation pressure is not more than 200pa, and collecting fractions at corresponding temperatures to respectively obtain colorless and transparent monomers and solvents.

The degradable medical supplies are heated and dissolved in the reaction kettle to obtain the degradable materials and the coloring agent, the degradable materials, the coloring agent and the solvent form a homogeneous solution, the degradable materials are subjected to cracking reaction in the reaction kettle under the action of the catalyst to generate monomers, the coloring agent and the solvent are co-distilled out of the reaction kettle through reduced pressure distillation, and a mixed liquid is obtained through condensation and relatively directly cracked, the cracking and stirring resistance of a solution phase is small, the mass and heat transfer is more uniform, the influence of nonuniform local heating in direct cracking on the product quality can be effectively avoided, meanwhile, the monomers and the solvent form a homogeneous solution to co-distillate, the monomers can be prevented from being solidified and blocking a pipeline after contacting with the pipe wall and being cooled, and the industrial production can be realized more favorably; and the molecular chain of the polymer in the solution is fully stretched and moved, which is beneficial to increasing the contact area of the polymer and the catalyst and improving the reaction efficiency. And performing secondary reduced pressure distillation on the mixed liquid by using a rotary evaporator to respectively obtain a colorless and transparent monomer, a solvent and a coloring agent, thereby realizing the recovery of the degradable medical supplies. The monomer and the coloring agent are recovered by the method, the recovery rate is 75-86%, and the purity of the monomer can reach more than 99%. The recovered monomer and the coloring agent can be repeatedly utilized, the resource waste is avoided, the production cost of medical supplies is reduced, and meanwhile, the separated solvent can also be recycled for homogeneous phase cracking of materials.

In one embodiment, in step S1, the degradable medical supplies, the solvent, and the catalyst are respectively in parts by weight: 100 parts of degradable medical supplies, 20-200 parts of solvent and 0.1-5 parts of catalyst.

In one embodiment, in step S1, the degradable medical product is absorbable ligature clip, suture or other medical product made of polydioxanone, colorant.

In one embodiment, in step S1, the solvent is an aromatic ester compound with a boiling point of 300 ℃ to 410 ℃, and the aromatic ester compound is miscible with the degradable medical article under heating. Specifically, the solvent is dimethoxyethyl phthalate (DMEP), dibutyl phthalate (DBP), diethylene glycol dibenzoate (DEDB). Preferably, the solvent is dimethoxyethyl phthalate. The dimethoxy ethyl phthalate can be mutually dissolved with the degradable material after being heated to form a homogeneous solution, and can also form a homogeneous solution with the monomer at normal temperature. Compared with direct cracking, the mass transfer and heat transfer of the cracking reaction of the solution phase are more uniform, the influence of nonuniform local heating caused by direct cracking on the product quality can be effectively avoided, and the monomer and the solvent form a homogeneous solution to be co-distilled off, so that the monomer can be prevented from being solidified and blocking a pipeline after being contacted with the pipe wall for cooling.

In one embodiment, in step S2, the colorant is solvent violet 13, solvent violet 9, solvent yellow 93, or other colorant with a boiling point above 450 ℃.

In one embodiment, in step S1, the catalyst is one or more of copper oxide, niobium pentoxide, or other transition metal oxides, or one or more of attapulgite, or other clay-based catalysts, preferably copper oxide. The catalyst can promote the cracking of the degradable material, effectively improve the recovery speed of the degradable material, shorten the reaction time and reduce the reaction temperature.

Implementation scenarios

Example 1

Putting 100 parts of ligation clip, 20 parts of dimethoxy ethyl phthalate and 0.1 part of copper oxide into a reaction kettle, vacuumizing the kettle, and stopping vacuumizing when the pressure in the kettle is reduced to 1500 pa; heating the reaction kettle, and stirring the materials in the kettle at a rotating speed of 50r/min when the temperature in the kettle is raised to 110 ℃; when the temperature in the kettle rises to 190 ℃, the reaction time is calculated, the reaction is carried out for 20min, and materials in the kettle are condensed and refluxed in the reaction process; after the reaction is finished, vacuumizing the kettle, carrying out reduced pressure distillation on the materials in the reaction kettle, distilling out monomer dioxanone (PDO), dimethoxyethyl phthalate and solvent purple 13 from the reaction kettle, and condensing to obtain a mixed liquid; and (2) carrying out secondary reduced pressure distillation on the mixed liquid, wherein the distillation temperature is 60 ℃, the distillation rotation speed is 60r/min, the distillation pressure is 150pa, collecting fractions at the temperature to obtain colorless and transparent monomer dioxanone (PDO), the net yield is 85.3%, the purity is 99.68%, replacing the collection bottle after no fractions are generated, continuously heating to 200 ℃, collecting fractions at the temperature to obtain a reaction solvent, dissolving and filtering residual substances in the distillation bottle by ethyl acetate after the solvent is collected, carrying out reduced pressure distillation on the filtrate at 35 ℃ and 80pa, and washing and drying a solid product in the distillation bottle by clear water to obtain the solvent purple 13.

Example 2

Putting 100 parts of suture, 100 parts of dimethoxyethyl phthalate and 1 part of niobium pentoxide into a reaction kettle, vacuumizing the kettle, and stopping vacuumizing when the pressure in the kettle is reduced to 2000 pa; heating the reaction kettle, and stirring the materials in the kettle at a rotating speed of 200r/min when the temperature in the kettle is raised to 120 ℃; when the temperature in the kettle rises to 210 ℃, the reaction time is calculated, the reaction is carried out for 70min, and materials in the kettle are condensed and refluxed in the reaction process; after the reaction is finished, vacuumizing the reactor, carrying out reduced pressure distillation on the materials in the reactor, co-distilling PDO, dimethoxyethyl phthalate and solvent yellow 93 out of the reactor, and condensing to obtain a mixed liquid; and (2) carrying out secondary reduced pressure distillation on the mixed liquid, wherein the distillation temperature is 80 ℃, the distillation rotation speed is 80r/min, the distillation pressure is 100pa, collecting fractions at the temperature to obtain colorless and transparent PDO, the yield is 85.5%, the purity is 99.29%, after no fractions are generated, replacing a collection bottle, continuously heating to 190 ℃, collecting fractions at the temperature to obtain a reaction solvent, after the solvent is collected, dissolving and filtering residual substances in the distillation bottle by ethyl acetate, distilling the filtrate under reduced pressure at 30 ℃ and 75pa, washing a solid product in the distillation bottle by clear water, and drying to obtain a solvent yellow 93.

Example 3: putting 100 parts of suture, 200 parts of diethylene glycol dibenzoate and 5 parts of copper oxide into a reaction kettle, vacuumizing the kettle, and stopping vacuumizing when the pressure in the kettle is reduced to 1000 pa; heating the reaction kettle, and stirring the materials in the kettle at a rotating speed of 500r/min when the temperature in the kettle is raised to 130 ℃; when the temperature in the kettle rises to 250 ℃, the reaction time is calculated, the reaction is carried out for 120min, and materials in the kettle are condensed and refluxed in the reaction process; after the reaction is finished, vacuumizing the kettle, carrying out reduced pressure distillation on materials in the reaction kettle, co-distilling PDO, diethylene glycol dibenzoate and solvent purple 9 from the reaction kettle, and condensing to obtain a mixed liquid; and (2) carrying out secondary reduced pressure distillation on the mixed liquid, wherein the distillation temperature is 95 ℃, the distillation rotation speed is 100r/min, the distillation pressure is 110pa, collecting fractions at the temperature to obtain colorless and transparent PDO, the yield is 85.9%, the purity is 98.36%, after no fractions are generated, replacing a collection bottle, continuously heating to 195 ℃, collecting fractions at the temperature to obtain a reaction solvent, after the solvent is collected, dissolving and filtering residual substances in the distillation bottle by ethyl acetate, distilling the filtrate under reduced pressure at 40 ℃ and 100pa, and washing and drying a solid product in the distillation bottle by clear water to obtain the solvent purple 9.

Example 4: putting 100 parts of ligation clip, 20 parts of dibutyl phthalate and 1.5 parts of attapulgite into a reaction kettle, vacuumizing the kettle, and stopping vacuumizing when the pressure in the kettle is reduced to 800 pa; heating the reaction kettle, and stirring the materials in the kettle at a rotating speed of 90r/min when the temperature in the kettle is raised to 110 ℃; when the temperature in the kettle rises to 220 ℃, the reaction time is calculated, the reaction is carried out for 40min, and materials in the kettle are condensed and refluxed in the reaction process; after the reaction is finished, vacuumizing the reaction kettle, carrying out reduced pressure distillation on materials in the reaction kettle, co-distilling PDO, dibutyl phthalate and solvent purple 13 out of the reaction kettle, and condensing to obtain a mixed liquid; and (2) carrying out secondary reduced pressure distillation on the mixed liquid, wherein the distillation temperature is 75 ℃, the distillation rotation speed is 60r/min, the distillation pressure is 90pa, collecting fractions at the temperature to obtain colorless and transparent PDO, the net yield is 80.2%, the purity is 98.68%, after no fractions are generated, replacing a collecting bottle, continuously heating to 200 ℃, collecting fractions at the temperature to obtain a reaction solvent, after the solvent is collected, dissolving and filtering residual substances in the distilling bottle by ethyl acetate, distilling filtrate at 32 ℃ and 85pa under reduced pressure, and washing and drying a solid product in the distilling bottle by clear water to obtain the solvent purple 13.

Example 5: putting 100 parts of ligation clip, 150 parts of dimethoxy ethyl phthalate and 0.5 part of activated clay into a reaction kettle, vacuumizing the kettle, and stopping vacuumizing when the pressure in the kettle is reduced to 1600 pa; heating the reaction kettle, and stirring the materials in the kettle at a rotating speed of 100r/min when the temperature in the kettle is raised to 110 ℃; when the temperature in the kettle rises to 230 ℃, calculating the reaction time, reacting for 10min to obtain a material monomer PDO, and condensing and refluxing the material in the kettle in the reaction process; after the reaction is finished, vacuumizing the reactor, carrying out reduced pressure distillation on the materials in the reactor, co-distilling PDO, dimethoxyethyl phthalate and the solvent purple 13 out of the reactor, and condensing to obtain a mixed liquid; and (2) carrying out secondary reduced pressure distillation on the mixed liquid, wherein the distillation temperature is 70 ℃, the distillation rotation speed is 60r/min, the distillation pressure is 180pa, collecting fractions at the temperature to obtain colorless and transparent PDO, the net yield is 85.3%, the purity is 99.18%, after no fractions are generated, replacing a collection bottle, continuously heating to 210 ℃, collecting fractions at the temperature to obtain a reaction solvent, after the solvent is collected, dissolving and filtering residual substances in the distillation bottle by ethyl acetate, distilling the filtrate under reduced pressure at 30 ℃ and 70pa, and washing and drying a solid product in the distillation bottle by clear water to obtain the solvent purple 13.

Example 6: the solvent dimethoxyethyl phthalate recovered from example 5 was used for depolymerization of the degraded material. Putting 100 parts of ligation clip, 100 parts of dimethoxyethyl phthalate and 2 parts of activated clay into a reaction kettle, vacuumizing the kettle, and stopping vacuumizing when the pressure in the kettle is reduced to 1200 pa; heating the reaction kettle, and stirring the materials in the kettle at a rotating speed of 200r/min when the temperature in the kettle is raised to 120 ℃; when the temperature in the kettle rises to 200 ℃, the reaction time is calculated, the reaction is carried out for 100min, and materials in the kettle are condensed and refluxed in the reaction process; after the reaction is finished, vacuumizing the reactor, carrying out reduced pressure distillation on the materials in the reactor, co-distilling PDO, dimethoxyethyl phthalate and the solvent purple 13 out of the reactor, and condensing to obtain a mixed liquid; and (2) carrying out secondary reduced pressure distillation on the mixed liquid, wherein the distillation temperature is 70 ℃, the distillation rotation speed is 80r/min, the distillation pressure is 80pa, collecting fractions at the temperature to obtain colorless and transparent PDO, the net yield is 80.8%, the purity is 98.27%, after no fractions are generated, replacing a collecting bottle, continuously heating to 185 ℃, collecting fractions at the temperature to obtain a reaction solvent, after the solvent is collected, dissolving and filtering residual substances in the distilling bottle by using ethanol, distilling filtrate at 36 ℃ and 88pa under reduced pressure, and washing and drying a solid product in the distilling bottle by using clear water to obtain the solvent purple 13.

Please refer to fig. 2-6, which are schematic diagrams of the recycling process of the absorbable ligature clamp. FIG. 2 is a schematic view of an absorbable ligature clip; FIG. 3 is a schematic view of a mixed liquid obtained by reacting an absorbable ligation clip in a reaction vessel and distilling the reaction vessel under reduced pressure; FIG. 4 is a schematic view of a recovered colorless transparent monomer; FIG. 5 is a schematic illustration of recovered solvent; fig. 6 is a schematic view of the recovered stain.

Referring to table 1, the yields of the monomer, the solvent and the stain were compared under different experimental conditions, and when the solvent was DEDB, the reaction temperature was 250 ℃, and the reaction pressure was 1000pa, the yield of the monomer was the highest, and 85.9%, and the yield of the stain was the highest, and 81.2%.

TABLE 1 Experimental results for the examples

Examples	Solvent(s)	Boiling point/. degree.C	Reaction temperature/. degree.C	Reaction pressure/Pa	Monomer yield/%	Solvent yield/%	Yield of coloring agent/%)
								1	DMEP	350	190	1500	85.3	90.3	77.5
2	DMEP	350	210	2000	85.5	92.5	78.4
								3	DEDB	408	250	1000	85.9	91.2	81.2
4	DBP	337	220	800	80.2	94.1	75.5
								5	DMEP	350	230	1600	85.3	90.1	79.2
6	DMEP	350	200	1200	80.8	89.6	78.3

While the above-described embodiments describe the method of recycling a degradable medical article in more detail, the following embodiments will attempt to briefly describe the apparatus for carrying out the method, i.e., the recycling apparatus for a degradable medical article.

Referring to fig. 7 to 8, the recycling device of a degradable medical product disclosed in the present application is used for recycling monomers and coloring agents in the degradable medical product. The recovery device comprises a reaction kettle 1 with a stirring mechanism 11 and a heating mechanism 12. The stirring mechanism 11 is used for stirring the materials in the reaction kettle 1. Heating mechanism 12 has heating jacket 13 and heat preservation 14, and heating jacket 13 is used for heating reation kettle 1, and heat preservation 14 is used for keeping warm to reation kettle 1, avoids calorific loss.

This recovery unit still includes:

and the collecting tank 2 is communicated with the reaction kettle 1 through a material pipe 3. Referring to fig. 1, one end of a material pipe 3 is connected to the top of the reaction vessel 1, and the other end extends to the upper part of the reaction vessel 1 and then is connected to a collection tank 2 while inclining downward. The material pipe 3 is provided with a first valve 31. After material pipe 3 extends to reation kettle 1's top part, the downward sloping again, the material in the reation kettle 1 of being convenient for is distilled the condensation back, flows into collection tank 2.

And one end of the return pipe 35 is communicated with the reaction kettle 1, and the other end of the return pipe 35 is communicated with one end of the material pipe 3 which is inclined downwards and is close to the collecting tank 2. A second valve 36 is arranged at one end of the return pipe 35 close to the material pipe 3, and a third valve 37 is arranged at one end close to the reaction kettle 1. The materials in the reaction kettle 1 are condensed and refluxed through a reflux pipe 35 in the reaction process.

And the vacuum mechanism 4 is communicated with the collection tank 2 through a vacuum pipe 42. The vacuum mechanism 4 is used for evacuating the collection tank 2 and the reaction kettle 1 to reduce the pressure in the collection tank 2 and the reaction kettle 1.

And the distillation equipment (not shown in the figure) is connected with the collecting tank 2, and the material in the collecting tank 2 enters the distillation equipment for distillation. The distillation equipment is a rotary evaporator and is used for distilling the materials collected in the collection tank 2 and recovering the material monomers and the coloring agent.

Wherein, the pipe wall outside that material pipe 3 downward sloping is equipped with condenser pipe 32. Both ends of the condensation duct 32 are provided with a condensation water inlet 33 and a condensation water outlet 34, respectively. The condensed water enters the condensation pipe 32 from the lower condensed water inlet 33, can condense the material in the material pipe 3 into liquid, flows into the collection tank 2, and is discharged out of the condensation pipe 32 from the upper condensed water outlet 34.

After the degradable medical supplies react in the reaction kettle 1 to generate the monomer and the coloring agent, the degradable medical supplies are subjected to reduced pressure distillation in the reaction kettle 1 under the evacuation action of the vacuum mechanism 4, enter the material pipe 3, are condensed by the condenser pipe 32 and then flow into the collection tank 2. And the materials in the collecting tank 2 are subjected to reduced pressure distillation by a distillation device, and the monomers and the coloring agent are respectively recovered.

The main raw materials of the degradable medical supplies are degradable materials and coloring agents, and after the degradable medical supplies react in the reaction kettle 1, monomers, the coloring agents and solvents can be separated from the reaction kettle 1 through reduced pressure distillation. And carrying out reduced pressure distillation on the monomer, the coloring agent and the solvent through a rotary evaporator to respectively obtain the monomer, the coloring agent and the solvent, so that the degradable medical supplies are recovered, and the recovery rate is 75-86%. The recovered monomer, coloring agent and solvent can be reused, so that resource waste is avoided, and the production cost of medical supplies is reduced.

In one embodiment, as shown in FIG. 7, the vacuum mechanism 4 has a buffer tank 41. The buffer tank 41 communicates with the collection tank 2 through a vacuum pipe 42. The buffer tank 41 is provided with a vacuum pump port 43 and a sewage drain pipe 44. The vacuum pump port 43 is located on the upper side of the buffer tank 41 and connected to a vacuum pump (not shown). The drain pipe 44 is located at the bottom of the buffer tank 41 and is provided with a fourth valve 45.

Specifically, one end of the vacuum tube 42 is connected to the top of the collection tank 2, and the other end extends into the buffer tank 41 from the top of the buffer tank 41 to the position below the vacuum pump opening 43, so that the vacuum pump is prevented from being damaged due to the fact that materials are pumped into the vacuum pump when the vacuum pump is emptied.

Can prevent through setting up buffer tank 41 that the vacuum pump from taking place to suck backward and entering into collecting vessel 2, play the cushioning effect to the evacuation simultaneously, prevent reaction system pressure shock.

In one embodiment, the collection tank 2 includes a drain pipe 21, a drain pipe 22, a manhole 23, and a collection pipe 24. The evacuation pipe 21 is provided at the top of the collection tank 2, is in communication with the atmosphere, and is provided with an exhaust valve 25. A discharge conduit 22 is arranged at the bottom of the collecting tank 2, on which a fifth valve 26 is arranged. A manhole 23 is provided at an upper side of the tank body of the collection tank 2 for observing the inside of the collection tank 2. Referring to figure 8, the collection tube 24 is connected at one end to the material tube 3 and extends inwardly from the top of the collection tank 2 to the viewing area of the manhole 23 at the other end. The liquid dropping from the collecting pipe 24 can be observed through the manhole 23, and whether the distillation is finished or not can be judged.

In one embodiment, the recycling apparatus further comprises a controller. The controller is connected with the heating mechanism 12, the stirring mechanism 11 and the vacuum mechanism 4 and can control the heating mechanism 12, the stirring mechanism 11 and the vacuum mechanism 4 to be switched on and off. The reaction kettle 1 is provided with a temperature sensor 16 and a pressure sensor 15, and the temperature sensor 16 and the pressure sensor 15 are connected with a controller. The controller can adjust the heating mechanism 12, the stirring mechanism 11 and the vacuum mechanism 4 according to the temperature and the pressure detected by the temperature sensor 16 and the pressure sensor 15.

In one embodiment, the recycling device further comprises an inlet pipe 17. Referring to fig. 7, one end of the gas inlet pipe 17 extends into the reaction kettle 1 to the bottom of the kettle body, and the other end is connected with an inert gas tank (not shown in the figure). The air inlet pipe 17 is used for introducing inert gas into the reaction kettle 1, so that the recovery device can be used for reaction in an inert gas atmosphere, and after the reaction is finished, the whole reaction kettle 1 can be purged and dried through the air inlet pipe 17 by using the inert gas.

In one embodiment, the recycling apparatus further includes a cooling tube 18. The cooling pipe 18 is located inside the reaction vessel 1, and has one end connected to a cooling water inlet of a cooling water tank (not shown) and the other end connected to a cooling water outlet. Cooling water in the cooling water tank enters the cooling pipe 18 through the cooling water outlet, the cooling pipe 18 cools the reaction kettle 1, and the cooling water enters the cooling water tank from the cooling water inlet.

The recovery device of the degradable medical supplies has the working modes that:

putting the degradable medical supplies, the solvent and the catalyst into a reaction kettle 1, starting a vacuum pump, vacuumizing the kettle to be below 2000pa, closing the vacuum pump, and starting a heating mechanism 12; when the temperature in the kettle rises to 110-130 ℃, starting the stirring mechanism 11, and stirring the materials in the kettle by the stirring mechanism 11 at a rotating speed of 50-500 r/min to dissolve the degradable medical supplies in the solvent to form a homogeneous solution of the polymer and the coloring agent; when the temperature in the kettle rises to 180-250 ℃, the reaction time is calculated, the reaction lasts for 10-120 min to obtain a monomer, and in the reaction process, materials in the kettle are condensed and refluxed through a reflux pipe 35; after the reaction is finished, the condensed water is opened, the vacuum pump is started, the materials in the reaction kettle 1 are subjected to reduced pressure distillation, the monomers, the coloring agent and the solvent are co-distilled out of the reaction kettle 1 and enter the material pipe 3, and the monomers, the coloring agent and the solvent flow into the collection tank 2 after being condensed by the condensed water in the condensation pipe 32; observing the collecting pipe 24 through the manhole 23, when the collecting pipe 24 does not produce liquid drops any more, closing the vacuum pump, opening the exhaust valve 25 to enable the system to be recovered to normal pressure, and closing the heating mechanism 12 and the stirring mechanism 11; when the temperature in the kettle is reduced to below 200 ℃, the cooling pipe 18 in the kettle is opened to accelerate the temperature reduction of the kettle body, and the kettle cover is opened after the temperature is reduced to below 100 ℃ to clean the kettle body and the stirring mechanism 11; and (3) putting the materials in the collecting tank 2 into a rotary evaporator for distillation to respectively obtain a colorless and transparent monomer, a coloring agent and a solvent.

The utility model provides a recovery unit can retrieve monomer and coloring agent among the degradable medical supplies, and degradable medical supplies heats in reation kettle 1 and melts, obtains degradable material and coloring agent, and degradable material, coloring agent and solvent form homogeneous phase solution, and degradable material takes place the reaction in reation kettle 1 and generates the monomer under the effect of catalyst, and monomer, coloring agent and solvent are distilled off from reation kettle 1 interior altogether through the vacuum distillation, and the condensation obtains the mixed liquor. And performing secondary reduced pressure distillation on the mixed liquid by using a rotary evaporator to respectively obtain a monomer, a coloring agent and a solvent, thereby realizing the recovery of the degradable material. The recycled monomer, the coloring agent and the solvent can be repeatedly utilized, so that the resource waste is avoided, and the production cost of the medical supplies is reduced.

The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims

1. A method for recycling a degradable medical article, comprising the steps of:

2. The method for recycling the degradable medical supplies according to claim 1, wherein in the step S1, the degradable medical supplies, the solvent and the catalyst are respectively prepared by the following steps: 100 parts of degradable medical supplies, 20-200 parts of solvent and 0.1-5 parts of catalyst.

3. The method for recycling the degradable medical supplies according to claim 1, wherein in the step S1, the degradable medical supplies are absorbable ligature clips, sutures or other medical products using polydioxanone, coloring agent as raw materials.

4. The method for recycling the degradable medical supplies according to claim 1, wherein in the step S1, the solvent is an aromatic ester compound with a boiling point of 300 ℃ to 410 ℃, and the aromatic ester compound is miscible with the degradable medical supplies under heating.

5. The method for recycling the degradable medical supplies according to claim 1, wherein the coloring agent in step S2 is solvent violet 13, solvent violet 9, solvent yellow 93 or other coloring agent with boiling point higher than 450 ℃.

6. The method for recycling the degradable medical supplies according to claim 1, wherein in the step S1, the catalyst is one or more of copper oxide, niobium pentoxide, attapulgite, activated clay or other transition metal oxide, and clay-based catalyst.

7. The utility model provides a recovery unit of degradable medical supplies for monomer and coloring agent among the recovery degradable medical supplies, including taking rabbling mechanism, heating mechanism's reation kettle, its characterized in that still includes:

wherein a condensing pipe is sleeved on the outer side of the pipe wall of the material pipe, which is inclined downwards; after the degradable medical supplies react in the reaction kettle to generate monomers and coloring agents, the degradable medical supplies are subjected to reduced pressure distillation in the reaction kettle under the vacuumizing action of the vacuum mechanism, enter the material pipe, are condensed by the condenser pipe and flow into the collection tank; and carrying out reduced pressure distillation on the materials in the collecting tank by using a distillation device, and respectively recovering the monomer, the solvent and the coloring agent.

8. The recycling device of degradable medical supplies according to claim 7, wherein the vacuum mechanism has a buffer tank, the buffer tank is communicated with the collection tank through the vacuum tube;

the sewage discharge pipe is positioned at the bottom of the buffer tank, and a fourth valve is arranged on the sewage discharge pipe;

9. The recycling apparatus of degradable medical supplies according to claim 7, wherein said collection tank comprises:

10. The recycling device of degradable medical supplies of claim 7, wherein said recycling device further comprises a controller; the controller is connected with the heating mechanism, the stirring mechanism and the vacuum mechanism;