CN217887963U - Hydrolysis reaction device for lactic acid oligomer cracking cyclization substrate - Google Patents
Hydrolysis reaction device for lactic acid oligomer cracking cyclization substrate Download PDFInfo
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- CN217887963U CN217887963U CN202220339110.0U CN202220339110U CN217887963U CN 217887963 U CN217887963 U CN 217887963U CN 202220339110 U CN202220339110 U CN 202220339110U CN 217887963 U CN217887963 U CN 217887963U
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Abstract
The utility model discloses a hydrolysis reaction device of lactic acid oligomer schizolysis cyclization substrate belongs to polylactic acid production technical field. Through the rotation of the spiral shell area and the body in the one-level converter hydrolysis reactor, in time with being thick form semifluid state's material transfer out in the upper reaches schizolysis cyclization reactor, both avoided schizolysis cyclization reactor to take place to solidify and/or coking phenomenon, guaranteed again that viscous material is intensive mixing and be heated evenly in the stove, effectively promote going on of one-level hydrolysis reaction, the material viscosity before finally getting into second grade hydrolysis reaction cauldron is by greatly reduced, the resistance of agitator stirring correspondingly reduces, the electric energy has been saved, simultaneously because the interior mass transfer of second grade hydrolysis reaction cauldron, the improvement of heat transfer, and the autocatalysis phenomenon that the acidity increase arouses, make second grade hydrolysis reaction will be more rapid and thorough. The utility model discloses a load adjustment elasticity is big, easy operation, equipment investment are little, energy-conserving, can effectively improve the utilization ratio of lactic acid or the total yield of lactide finally.
Description
Technical Field
The utility model belongs to the technical field of polylactic acid production, a hydrolysis reaction device of lactic acid oligomer schizolysis cyclization substrate is related to.
Background
The polylactic acid is a novel biodegradable polyester high molecular compound polymerized by using lactic acid as a monomer, can be hydrolyzed under the catalysis of enzymes or acids and bases in microorganisms or organisms to finally form carbon dioxide and water, realizes the circulation in the nature, is harmless and nontoxic to the human body, has no pollution to the environment, and is a degradable material with great development potential. In the aspect of application, polylactic acid can be applied to the field of medical and medical equipment materials, and also can be applied to the field of film products, such as agricultural mulching films, shopping bags, express delivery bags, packaging bags, freshness protection bags and the like, and can also be processed into downhole tool members for hydrocarbon resource recovery, temporary plugging agent materials and the like. Therefore, the polylactic acid serving as a novel degradable material has considerable economic benefits and good application prospects, and is an effective way for solving the problem of environmental pollution caused by plastic wastes and relieving the shortage of petroleum resources.
At present, two methods are mainly used for synthesizing polylactic acid: direct polycondensation of lactic acid and indirect polycondensation of lactic acid through the intermediate lactide. In the direct polycondensation method, since impurities exist in the system and the lactic acid polycondensation reaction is a reversible reaction, it is difficult to obtain polylactic acid having a high molecular weight. The indirect polycondensation method is used for synthesizing the polylactic acid, no special auxiliary agent is needed to be introduced, and the molecular weight of the product can reach hundreds of thousands or even millions. Therefore, the indirect polycondensation method is the most globally used polylactic acid production method at present. However, the indirect polycondensation process is lengthy, the reaction conditions are severe, and the requirements for equipment are high. Particularly, when the lactic acid raw material is cracked into gas-phase lactide generated by a loop reactor, lactic acid cannot be completely converted into lactide, a part of lactic acid oligomer with higher molecular weight is generated, and side reactions such as high-temperature oxidation and carbonization also occur. These side reaction products are usually dark brown viscous liquids, and as the viscosity of the material system increases, if the material system cannot be discharged in time, the solidification and/or coking at the bottom of the reaction kettle can be caused, so that the pipeline blockage is caused, and the yield and the purity of the lactide are seriously influenced. Generally, in a single-pass conversion of lactic acid to lactide, there is 30% conversion to substrate, which if discarded increases the raw material cost for lactide production and causes environmental damage. Therefore, there is a strong need in the art to provide a highly efficient method for hydrolyzing lactic acid oligomers to cleave cyclized substrates, thereby increasing the overall yield of lactide and reducing environmental pollution.
SUMMERY OF THE UTILITY MODEL
The utility model aims to overcome the shortcomings of the prior art and provide a hydrolysis reaction device for the lactic acid oligomer cracking cyclization substrate.
In order to achieve the above purpose, the utility model adopts the following technical scheme to realize: a hydrolysis reaction device of lactic acid oligomer cracking cyclization substrate comprises a primary converter hydrolysis reactor, a secondary hydrolysis reaction kettle, a liquid filter and a falling film evaporator;
the feed end of the primary converter hydrolysis reactor is provided with a feed inlet, a cracking cyclization substrate pipeline, a lactic acid prepolymerization process evaporation water pipeline and an outlet of a reflux water pump, the discharge end of the primary converter hydrolysis reactor is provided with a discharge outlet, the feed pipeline of the secondary hydrolysis reactor is connected, the outer side of the discharge end is also provided with a # 2 heating sleeve, and the # 2 heating sleeve is communicated with the # 1 heating sleeve through a pipeline so as to prevent the material from being solidified and forming blockage;
a stirrer, a feeding pipe, a coil heater and an overflow weir are arranged in the secondary hydrolysis reaction kettle; the stirrer is connected with a No. 2 driving motor and drives the stirrer to rotate and stir; the inlet of the feeding pipe is connected with the outlet of the discharge end of the primary converter hydrolysis reactor, and the outlet of the feeding pipe is inserted into the bottom of the secondary hydrolysis reactor and is close to the bottom surface; the coil heater is positioned below the liquid level of the secondary hydrolysis reaction kettle to provide heat for the hydrolysis reaction; the overflow weir is arranged at the upper part of the secondary hydrolysis reaction kettle, and the reaction liquid overflows out of the reaction kettle;
the inlet of the liquid filter is connected with the outlet of an overflow weir of the secondary hydrolysis reaction kettle, the solid-phase outlet of the liquid filter is connected with a waste solid pipeline, and the liquid-phase outlet of the liquid filter is connected with the upper liquid-phase inlet of the falling-film evaporator;
an outlet at the bottom of the falling-film evaporator is sequentially connected with an inlet of a No. 1 gas-liquid separator and an inlet of a circulating pump, and an outlet pipeline of the circulating pump is divided into two branches which are respectively connected with an upper liquid phase inlet of the falling-film evaporator and a hydrolysate pipeline; the gas phase outlet at the top of the 1# gas-liquid separator is sequentially connected with inlets of a first-stage condenser, a 2# gas-liquid separator, a second-stage condenser, a 3# gas-liquid separator and a vacuum pump, and the liquid phase outlet of the 3# gas-liquid separator is sequentially connected with inlets of the 2# gas-liquid separator and a reflux water pump.
Further, the primary converter hydrolysis reactor body is of a cylindrical structure, a No. 1 heating sleeve is arranged on the outer side of the primary converter hydrolysis reactor body, a rotating shaft is arranged along the axial direction of the primary converter hydrolysis reactor body and is connected with a No. 1 driving motor, the rotating shaft is driven by the No. 1 driving motor to further drive the primary converter hydrolysis reactor body and a spiral belt to rotate, and the spiral belt is spirally wound and distributed on a central shaft along the axial direction of the central shaft;
furthermore, the viscosity of the reaction liquid in the first-stage converter hydrolysis reactor is far greater than that of the reaction liquid in the second-stage hydrolysis reactor, and the fluidity of the reaction liquid is driven by a spiral belt; the viscosity of the reaction liquid in the secondary hydrolysis reaction kettle is far greater than that of the liquid in the falling film evaporator, and the stirrer adopts an anchor stirrer suitable for high-viscosity liquid to drive the fluidity of the high-viscosity liquid.
Furthermore, the secondary condenser adopts low-temperature refrigerant as a refrigerant, so that substances which are easy to solidify are prevented from entering the vacuum pump.
Further, the reaction product after being fully hydrolyzed by the primary converter hydrolysis reactor and the secondary hydrolysis reactor is dehydrated, and a falling film evaporator suitable for high-viscosity and high-heat sensitivity materials is adopted to carry out vacuum evaporation on the reaction product.
Furthermore, the reaction water injected into the first-stage converter hydrolysis reactor and the second-stage hydrolysis reactor respectively comes from the pipeline of the upstream lactic acid prepolymerization unit and the process distilled water of the falling film evaporator, and the water of the first-stage converter hydrolysis reactor and the process distilled water of the falling film evaporator contains a small amount of lactic acid and is acidic.
Compared with the prior art, the utility model discloses following beneficial effect has:
the utility model discloses a load adjustment elasticity is big, and the operation is thus simple, the equipment investment is little, energy-conservation, rotation through the spiral shell in the one-level converter hydrolysis reactor, in time with being thick form semifluid state's material transfer out in the cracking cyclization reactor of upper reaches, can effectively avoid the material to solidify and/or coking phenomenon because of the further aggravation of reaction degree cracking cyclization reactor taking place, the material that is thick form semifluid state advances under the drive of spiral shell, it can hydrolyze gradually in advancing process, and simultaneously, the rotation of furnace body can increase the homogeneity of being heated and promote the further mixing and the reaction of reaction material, the reaction liquid before finally getting into the second grade hydrolysis reaction cauldron is after the one-level hydrolysis reaction, its viscosity has greatly reduced, thereby reduced the resistance when anchor agitator stirs in the second grade hydrolysis reaction cauldron, the electric energy has been saved, simultaneously because the improvement of the heat transfer in the second grade hydrolysis reaction cauldron, the hydrolysis reaction will be more rapid and thorough, finally can effectively improve the yield of lactide, furthermore, in the lactic acid hydrolysis unit of upper reaches and the lactic acid process that falls all contain a small amount of lactic acid hydrolysis, consequently, the catalytic hydrolysis reaction cost has been reduced has been added and has been evaporated again to any lactic acid hydrolysis reaction substrate.
Drawings
FIG. 1 is a schematic diagram of the structure of a hydrolysis reactor for cracking and cyclizing a substrate by using lactic acid oligomers according to the present invention.
In the figure, a 1-second-stage hydrolysis reaction kettle; 2-coil heater; 3-an overflow weir; 4-a stirrer; 5-feeding pipe; 6-a first-stage converter hydrolysis reactor; 7-1# heating jacket; 8-helical ribbon; 9-a reflux water pump; 10-falling film evaporator; 11-a liquid filter; 12-1# gas-liquid separator; 13-a circulation pump; 14-a first-stage condenser; 15-2# gas-liquid separator; 16-a secondary condenser; 17-3# gas-liquid separator; 18-a vacuum pump; 19-2# heating mantle; 20-a discharge end; 21-a feed end; 22-1# drive motor; 23-a body; 24-a rotating shaft; 25-2# drive motor; 30-a tail gas pipeline; evaporating a water pipeline by a 31-lactic acid prepolymerization process; a 32-lactic acid oligomer cracking cyclization substrate pipeline; 33-spent solids pipeline; 34-hydrolysate conduit.
Detailed Description
In order to make the technical solution of the present invention better understood, the technical solution of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by a person skilled in the art without creative efforts shall fall within the protection scope of the present invention.
It should be noted that the terms "first," "second," and the like in the description and claims of the present invention and in the drawings described above are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used is interchangeable under appropriate circumstances such that the embodiments of the invention described herein are capable of operation in other sequences than those illustrated or described herein. Furthermore, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
The present invention will be described in further detail with reference to the accompanying drawings:
referring to fig. 1, fig. 1 is a schematic structural diagram of the present invention, a hydrolysis reaction apparatus for cracking cyclized substrate by lactic acid oligomer, comprising a primary converter hydrolysis reactor 7, a secondary hydrolysis reactor 1, a liquid filter 11, a falling film evaporator 10 and a vacuum pump 18. The viscous semi-fluid material from the upstream lactic acid oligomer cracking cyclization substrate pipeline 32 enters the first-stage converter hydrolysis reactor 6 through a feeding hole arranged at the feeding end 21 of the first-stage converter hydrolysis reactor 6, and meanwhile, the process distilled water containing a small amount of acidic lactic acid from the lactic acid prepolymerization process distilled water pipeline 31 and the outlet of the reflux water pump 9 is also added into the inlet of the feeding end 21 of the first-stage converter hydrolysis reactor 6.
The lactic acid oligomer cracking cyclization substrate belongs to a polyester compound, and can be subjected to hydrolysis reaction with water under the conditions of a certain temperature and a catalyst. The hydrolysis reaction process starts from the migration of water molecules to the surface of an oligomer, the water molecules gradually diffuse into the periphery of ester bonds or hydrophilic groups, and under the action of catalysts such as acid or alkali in a medium, the ester bonds are broken and form a carboxyl and a hydroxyl with water. The process of hydrolysis and chain scission gradually reduces the polymerization degree of the oligomer, and when the polymerization degree is reduced to a certain degree, the oligomer begins to dissolve to form hydrolysis products such as monomolecular lactic acid and lactic acid oligomer which can be dissolved in lactic acid solution.
After entering a first-stage converter hydrolysis reactor 6, lactic acid oligomer cracking cyclization substrate and water evaporated by the process enter a first-stage converter hydrolysis reactor 6, the lactic acid oligomer cracking cyclization substrate and the water are driven by a screw belt 8 to move forward, a body 23 of the first-stage converter hydrolysis reactor 6 is of a cylindrical structure, a 1# heating sleeve 7 is arranged on the outer side of the body to provide heat for hydrolysis reaction, meanwhile, the rotation of the furnace body 6 can increase the uniformity of heating and promote further mixing and reaction of reaction materials, when the materials move to a discharge port of a discharge end 20 of the first-stage converter hydrolysis reactor 6, the first-stage hydrolysis reaction is completed, the viscosity of the materials is greatly reduced, the acidity of the materials is further increased, meanwhile, a 2# heating sleeve 19 is also arranged on the outer side of the discharge end 20, and the 2# heating sleeve 19 is communicated with the 1# heating sleeve 7 through a pipeline so as to prevent the materials from being solidified and forming blockage.
Then, the reaction materials enter an inlet of a feed pipeline 5 of a second-stage hydrolysis reaction kettle 1 through an outlet of a discharge end 20 of a first-stage converter hydrolysis reactor 6, and an outlet of the feed pipeline 5 is inserted into the bottom of the second-stage hydrolysis reaction kettle 1 and is discharged close to the bottom surface; the coil heater 2 is positioned below the liquid level of the secondary hydrolysis reaction kettle 1 and provides heat required by the hydrolysis reaction; the overflow weir 3 is provided at the upper portion of the secondary hydrolysis reaction vessel 1, from which the reaction solution overflows out of the reaction vessel, and the height thereof determines the liquid holdup of the secondary hydrolysis reaction vessel 1, that is, the time of the secondary hydrolysis reaction.
After the material is subjected to primary hydrolysis by the primary converter hydrolysis reactor 6, the acidity of the material is further increased along with the generation of lactic acid, the acidity of the material is an important factor influencing the hydrolysis rate of a substrate for cracking and cyclizing lactic acid oligomer, and the rate of hydrolytic cleavage of an ester bond in an alkaline or acidic environment is higher than that in a neutral environment. Therefore, as the hydrolysis process proceeds, the amount of terminal carboxyl groups gradually increases, the hydrolysis rate increases, and the autocatalysis phenomenon occurs in the reaction, so that the secondary hydrolysis reaction kettle 1 does not need to add fresh lactic acid as a catalyst. At the same time, the more fully the water and oligomer are contacted, the more favorable the hydrolysis of the oligomer. In order to realize the full contact of two phases, aiming at the characteristic that the viscosity of the reaction materials is greatly reduced after the first-stage hydrolysis, the stirrer 4 of the second-stage hydrolysis reaction kettle 1 adopts a common anchor type stirring paddle, so that good mixing performance can be obtained, and the corresponding power consumption is effectively reduced due to the great reduction of the resistance.
After passing through the secondary hydrolysis reaction vessel 1, the hydrolysis reaction of the lactic acid oligomer cracking cyclization substrate is carried out completely, and the effective components in the lactic acid oligomer are hydrolyzed into soluble low molecular weight oligomers such as lactic acid dimer and trimer even if the lactic acid monomer cannot be hydrolyzed completely.
Finally, the reaction material is sent to a liquid filter 11 through an outlet of an overflow weir 3 of the secondary hydrolysis reaction kettle 1, after the unavailable oxidized carbide and the upstream catalyst residue are removed, the reaction material enters a falling film evaporator 10 which is suitable for processing high-viscosity and high-heat-sensitivity materials to carry out vacuum evaporation on the reaction material, the water in the reaction material is removed, and the recyclable lactic acid is obtained, and the main components of the recyclable lactic acid comprise lactic acid, lactic acid dimer, lactic acid trimer and the like.
The process water evaporated by the falling-film evaporator 10 is recovered by two-stage condensation and returned to the first-stage converter hydrolysis reactor 6 again to be used as a hydrolysis reaction raw material. It should be noted that the secondary condenser 16 uses low-temperature refrigerant as refrigerant to prevent easily solidified substances from entering the vacuum pump 18, thereby protecting the vacuum pump 18.
The analysis can show that the hydrolysis reaction device for cracking and cyclizing the substrate by the lactic acid oligomer has the characteristics of ingenious design, small total occupied area, land acquisition saving, engineering investment reduction, energy conservation, simple operation, large load adjustment elasticity, safety, reliability and the like, and can be applied to engineering; and provides a new optimized solution structure for the technical field of polylactic acid production.
The above contents are only for explaining the technical idea of the present invention, and the protection scope of the present invention cannot be limited thereby, and any modification made on the basis of the technical solution according to the technical idea of the present invention all fall within the protection scope of the claims of the present invention.
Claims (6)
1. A hydrolysis reaction device of lactic acid oligomer cracking cyclization substrate comprises a primary converter hydrolysis reactor (6), a secondary hydrolysis reaction kettle (1), a liquid filter (11) and a falling film evaporator (10);
the device is characterized in that a feeding port is formed in a feeding end (21) of a first-stage converter hydrolysis reactor (6), a cracking cyclization substrate pipeline (32), a lactic acid prepolymerization process evaporation water pipeline (31) and an outlet of a reflux water pump (9) are connected, a discharging port is formed in a discharging end (20), a feeding pipe (5) of a second-stage hydrolysis reactor (1) is connected, a 2# heating sleeve (19) is also arranged on the outer side of the discharging end (20), and the 2# heating sleeve (19) is communicated with a 1# heating sleeve (7) through a pipeline so as to prevent materials from being solidified and blocked;
a stirrer (4), a feeding pipe (5), a coil heater (2) and an overflow weir (3) are arranged in the secondary hydrolysis reaction kettle (1); the stirrer (4) is connected with a 2# driving motor (25) to drive the stirrer (4) to rotate and stir; the inlet of the feeding pipe (5) is connected with the outlet of the discharge end (20) of the first-stage converter hydrolysis reactor (6), and the outlet of the feeding pipe is inserted into the bottom of the second-stage hydrolysis reaction kettle (1) and is close to the bottom surface; the coil heater (2) is positioned below the liquid level of the secondary hydrolysis reaction kettle (1) and provides heat for the hydrolysis reaction; the overflow weir (3) is arranged at the upper part of the secondary hydrolysis reaction kettle (1), and the reaction liquid overflows out of the reaction kettle;
the inlet of the liquid filter (11) is connected with the outlet of an overflow weir (3) of the secondary hydrolysis reaction kettle (1), the solid phase outlet of the liquid filter is connected with a waste solid pipeline (33), and the liquid phase outlet of the liquid filter is connected with the upper liquid phase inlet of the falling film evaporator (10);
an outlet at the bottom of the falling-film evaporator (10) is sequentially connected with a No. 1 gas-liquid separator (12) and an inlet of a circulating pump (13), and an outlet pipeline of the circulating pump (13) is divided into two branches which are respectively connected with a liquid phase inlet at the upper part of the falling-film evaporator (10) and a hydrolysate pipeline (34); a gas-phase outlet at the top of the 1# gas-liquid separator (12) is sequentially connected with inlets of a first-stage condenser (14), a 2# gas-liquid separator (15), a second-stage condenser (16), a 3# gas-liquid separator (17) and a vacuum pump (18), and a liquid-phase outlet of the 3# gas-liquid separator (17) is sequentially connected with inlets of the 2# gas-liquid separator (15) and a reflux water pump (9).
2. The hydrolysis reaction device for the cleavage and cyclization substrate of lactic acid oligomer according to claim 1, wherein the body (23) of the first-stage converter hydrolysis reactor (6) is cylindrical, a 1# heating jacket (7) is disposed on the outer side of the first-stage converter hydrolysis reactor, a rotating shaft (24) is disposed along the axial direction of the body (23), the rotating shaft is connected with a 1# driving motor (22), the rotating shaft (24) is driven by the 1# driving motor (22) to further drive the body (23) and the ribbon (8) to rotate, and the ribbon (8) is spirally wound along the axial direction of the central shaft and disposed on the central shaft.
3. The hydrolysis reaction device for the cleavage and cyclization substrate of lactic acid oligomer as claimed in claim 2, wherein the viscosity of the reaction solution in said primary converter hydrolysis reactor (6) is much higher than the viscosity of the reaction solution in said secondary hydrolysis reactor (1), and the fluidity of said reaction solution is driven by a ribbon (8); the viscosity of reaction liquid in the secondary hydrolysis reaction kettle (1) is far greater than that of liquid in the falling film evaporator (10), and the stirrer (4) adopts an anchor stirrer suitable for high-viscosity liquid to drive the fluidity of the high-viscosity liquid.
4. The hydrolysis reaction apparatus for the cleavage and cyclization substrate of lactic acid oligomer as claimed in claim 1, wherein said secondary condenser (16) uses a low temperature refrigerant as a refrigerant to prevent easily solidifiable substances from entering into said vacuum pump (18).
5. The hydrolysis reactor of the substrate for cleavage and cyclization of lactic acid oligomers as claimed in claim 1, wherein the dehydration of the reaction product after passing through the first stage converter hydrolysis reactor (6) and the second stage hydrolysis reactor (1) is carried out by vacuum evaporation using a falling film evaporator (10) suitable for high viscosity and high thermal sensitivity materials.
6. The hydrolysis reaction apparatus for the cleavage and cyclization substrate of lactic acid oligomer according to claim 1, wherein the reaction water injected into the primary converter hydrolysis reactor (6) and the secondary hydrolysis reactor (1) is respectively discharged from the pipeline (31) of the upstream lactic acid prepolymerization unit and the process water discharged from the falling film evaporator (10), and both of them contain a small amount of lactic acid and are acidic.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114471434A (en) * | 2022-02-18 | 2022-05-13 | 华陆工程科技有限责任公司 | Hydrolysis reaction device for lactic acid oligomer cracking cyclization substrate |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114471434A (en) * | 2022-02-18 | 2022-05-13 | 华陆工程科技有限责任公司 | Hydrolysis reaction device for lactic acid oligomer cracking cyclization substrate |
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