CN114405434A - Micro-interface system and method for preparing polybutylene succinate - Google Patents
Micro-interface system and method for preparing polybutylene succinate Download PDFInfo
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- CN114405434A CN114405434A CN202210201602.8A CN202210201602A CN114405434A CN 114405434 A CN114405434 A CN 114405434A CN 202210201602 A CN202210201602 A CN 202210201602A CN 114405434 A CN114405434 A CN 114405434A
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- 238000000034 method Methods 0.000 title claims description 8
- -1 polybutylene succinate Polymers 0.000 title abstract description 12
- 229920002961 polybutylene succinate Polymers 0.000 title abstract description 9
- 239000004631 polybutylene succinate Substances 0.000 title abstract description 9
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 claims abstract description 37
- 238000005886 esterification reaction Methods 0.000 claims abstract description 34
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000003054 catalyst Substances 0.000 claims abstract description 22
- 230000032050 esterification Effects 0.000 claims abstract description 19
- 238000006068 polycondensation reaction Methods 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 13
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 claims abstract description 11
- 239000001384 succinic acid Substances 0.000 claims description 10
- ZMKVBUOZONDYBW-UHFFFAOYSA-N 1,6-dioxecane-2,5-dione Chemical compound O=C1CCC(=O)OCCCCO1 ZMKVBUOZONDYBW-UHFFFAOYSA-N 0.000 claims description 7
- 238000004891 communication Methods 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 9
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- 239000007791 liquid phase Substances 0.000 abstract description 8
- 238000009826 distribution Methods 0.000 abstract description 3
- 239000006185 dispersion Substances 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 12
- 239000007788 liquid Substances 0.000 description 11
- 239000000047 product Substances 0.000 description 8
- 239000007789 gas Substances 0.000 description 7
- 239000000203 mixture Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 238000004806 packaging method and process Methods 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- FALRKNHUBBKYCC-UHFFFAOYSA-N 2-(chloromethyl)pyridine-3-carbonitrile Chemical compound ClCC1=NC=CC=C1C#N FALRKNHUBBKYCC-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 229920003232 aliphatic polyester Polymers 0.000 description 1
- 239000004621 biodegradable polymer Substances 0.000 description 1
- 229920002988 biodegradable polymer Polymers 0.000 description 1
- 238000006065 biodegradation reaction Methods 0.000 description 1
- CDQSJQSWAWPGKG-UHFFFAOYSA-N butane-1,1-diol Chemical compound CCCC(O)O CDQSJQSWAWPGKG-UHFFFAOYSA-N 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 1
- 239000012567 medical material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000012643 polycondensation polymerization Methods 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229940014800 succinic anhydride Drugs 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0093—Microreactors, e.g. miniaturised or microfabricated reactors
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/009—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in combination with chemical reactions
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/16—Dicarboxylic acids and dihydroxy compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
- C08G63/785—Preparation processes characterised by the apparatus used
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Polyesters Or Polycarbonates (AREA)
Abstract
The invention provides a micro-interface system for preparing polybutylene succinate, which comprises a mixing tank for premixing succinic acid, 1, 4-butanediol and a catalyst, wherein the mixing tank is connected with an esterification reactor, a linkage type micro-interface generator is arranged in the esterification reactor, the linkage type micro-interface generator is connected with a circulating pump, and a rectifying tower and a vacuum polycondensation tower are sequentially connected behind the esterification reactor. Through the inside at esterification reactor is provided with linkage micro-interface generator, with succinic acid, 1, 4 butanediol and catalyst dispersion breakage, can make succinic acid, 1, 4 butanediol and catalyst mutually dissolve better like this, solution temperature, concentration distribution are more even, have greatly strengthened the torrent degree of solution moreover for solid-liquid phase boundary layer further thins, increases substantially reaction efficiency, has practiced thrift manufacturing cost, improves production efficiency and output ratio.
Description
Technical Field
The invention belongs to the technical field of high polymer materials, and particularly relates to a micro-interface system and a method for preparing polybutylene succinate.
Background
Poly (butylene succinate) (PBS) is prepared by condensation polymerization of succinic acid and butanediol, has wide monomer source, is prepared without depending on petroleum resources, and can also be prepared by a biological fermentation method. PBS is a typical semicrystalline thermoplastic aliphatic polyester plastic, has good biodegradability and excellent mechanical properties, is between polyethylene and polypropylene, has good transparency, glossiness and printing performance and excellent forming processability, and is a green environment-friendly high-molecular polyester material with wide application prospect in artificially synthesized biodegradable materials.
The PBS can be applied to the field of national civilization such as packaging materials, disposable environment-friendly products, agricultural and forestry products, daily sundries, medical materials and the like. With the improvement of the living standard and environmental protection consciousness of people, the biodegradable environment-friendly nontoxic material is used in daily necessities such as the field of heat-resistant packaging products instead of the traditional material and has a trend. However, most biodegradable polymer materials have a heat resistance temperature lower than 90 ℃, and the heat distortion temperature of PBS is 69-80 ℃, which cannot meet the heat resistance requirement of heat-resistant packaging products. Therefore, the heat resistance of the current commercial PBS is necessary to be improved while the biodegradation performance and the mechanical performance of the PBS material are maintained, the application field of the PBS can be widened, and a new market can be developed.
At present, succinic anhydride is directly obtained after maleic anhydride is hydrogenated, succinic acid can be obtained through hydrolysis, hydrolysis water needs to be removed during esterification and polycondensation, energy consumption is high, sewage quantity is large, intermediate reaction products are excessive, and the problems of large sewage quantity, low esterification reaction activity and low production efficiency in the reaction process exist.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The invention aims to provide a micro-interface system for preparing polybutylene succinate, which is characterized in that a linked micro-interface generator is arranged in an esterification reactor to disperse and crush succinic acid, 1, 4-butanediol and a catalyst, so that the succinic acid, the 1, 4-butanediol and the catalyst can be better dissolved mutually, the solution temperature and the concentration are more uniformly distributed, the turbulence degree of the solution is greatly enhanced, a solid-liquid phase boundary layer is further thinned, the reaction efficiency is greatly improved, the production cost is saved, and the production efficiency and the output ratio are improved.
The second purpose of the invention is to provide a micro-interface method for preparing poly (butylene succinate), which is simple and convenient to operate and has high reaction efficiency.
In order to achieve the technical purpose, the invention provides the following technical scheme:
the invention provides a micro-interface system for preparing polybutylene succinate, which comprises a mixing tank for premixing succinic acid, 1, 4-butanediol and a catalyst, wherein the mixing tank is connected with an esterification reactor, a linkage type micro-interface generator is arranged in the esterification reactor, the linkage type micro-interface generator is connected with a circulating pump, and a rectifying tower and a vacuum polycondensation tower are sequentially connected behind the esterification reactor.
Preferably, the linkage type micro-interface generator comprises a hydraulic type micro-interface generator and a pneumatic type micro-interface generator.
Preferably, the hydraulic micro-interface generator is arranged right above the pneumatic micro-interface generator.
The linked micro-interface generator is arranged, so that succinic acid, 1, 4-butanediol and the catalyst can be dispersed and crushed, the succinic acid, 1, 4-butanediol and the catalyst can be better dissolved mutually, the solution temperature and concentration distribution are more uniform, the turbulence degree of the solution is greatly enhanced, the solid-liquid phase boundary layer is further thinned, the reaction efficiency is greatly improved, the production cost is saved, and the production efficiency and the output ratio are improved. The hydraulic micro-interface generator is arranged right above the pneumatic micro-interface generator because the pneumatic micro-interface generator can block the micro-pores due to the catalyst, and the material discharged from the hydraulic micro-interface generator is dispersed in the catalyst in the pores of the pneumatic micro-interface generator through the communicating pipeline, so that the stable reaction can be ensured.
Preferably, the device further comprises a communication pipeline, and the communication pipeline is connected with the hydraulic micro-interface generator and the pneumatic micro-interface generator.
It will be appreciated by those skilled in the art that the micro-interface generator used in the present invention is described in the prior patents of the present inventor, such as the patents of application numbers CN201610641119.6, CN201610641251.7, CN201710766435.0, CN106187660, CN105903425A, CN109437390A, CN205833127U and CN 207581700U. The detailed structure and operation principle of the micro bubble generator (i.e. micro interface generator) is described in detail in the prior patent CN201610641119.6, which describes that "the micro bubble generator comprises a body and a secondary crushing member, wherein the body is provided with a cavity, the body is provided with an inlet communicated with the cavity, the opposite first end and second end of the cavity are both open, and the cross-sectional area of the cavity decreases from the middle of the cavity to the first end and second end of the cavity; the secondary crushing member is disposed at least one of the first end and the second end of the cavity, a portion of the secondary crushing member is disposed within the cavity, and an annular passage is formed between the secondary crushing member and the through holes open at both ends of the cavity. The micron bubble generator also comprises an air inlet pipe and a liquid inlet pipe. "the specific working principle of the structure disclosed in the application document is as follows: liquid enters the micro-bubble generator tangentially through the liquid inlet pipe, and gas is rotated at a super high speed and cut to break gas bubbles into micro-bubbles at a micron level, so that the mass transfer area between a liquid phase and a gas phase is increased, and the micro-bubble generator in the patent belongs to a pneumatic micro-interface generator.
In addition, the first patent 201610641251.7 describes that the primary bubble breaker has a circulation liquid inlet, a circulation gas inlet and a gas-liquid mixture outlet, and the secondary bubble breaker communicates the feed inlet with the gas-liquid mixture outlet, which indicates that the bubble breakers all need to be mixed with gas and liquid, and in addition, as can be seen from the following drawings, the primary bubble breaker mainly uses the circulation liquid as power, so that the primary bubble breaker belongs to a hydraulic micro-interface generator, and the secondary bubble breaker simultaneously introduces the gas-liquid mixture into an elliptical rotating ball for rotation, thereby realizing bubble breaking in the rotating process, so that the secondary bubble breaker actually belongs to a gas-liquid linkage micro-interface generator. In fact, the micro-interface generator is a specific form of the micro-interface generator, whether it is a hydraulic micro-interface generator or a gas-liquid linkage micro-interface generator, however, the micro-interface generator adopted in the present invention is not limited to the above forms, and the specific structure of the bubble breaker described in the prior patent is only one of the forms that the micro-interface generator of the present invention can adopt.
Furthermore, the prior patent 201710766435.0 states that the principle of the bubble breaker is that high-speed jet flows are used to achieve mutual collision of gases, and also states that the bubble breaker can be used in a micro-interface strengthening reactor to verify the correlation between the bubble breaker and the micro-interface generator; moreover, in the prior patent CN106187660, there is a related description on the specific structure of the bubble breaker, see paragraphs [0031] to [0041] in the specification, and the accompanying drawings, which illustrate the specific working principle of the bubble breaker S-2 in detail, the top of the bubble breaker is a liquid phase inlet, and the side of the bubble breaker is a gas phase inlet, and the liquid phase coming from the top provides the entrainment power, so as to achieve the effect of breaking into ultra-fine bubbles, and in the accompanying drawings, the bubble breaker is also seen to be of a tapered structure, and the diameter of the upper part is larger than that of the lower part, and also for better providing the entrainment power for the liquid phase.
Since the micro-interface generator was just developed in the early stage of the prior patent application, the micro-interface generator was named as a micro-bubble generator (CN201610641119.6), a bubble breaker (201710766435.0) and the like in the early stage, and is named as a micro-interface generator in the later stage along with the continuous technical improvement, and the micro-interface generator in the present invention is equivalent to the micro-bubble generator, the bubble breaker and the like in the prior art, and has different names. In summary, the micro-interface generator of the present invention belongs to the prior art.
Preferably, the outlet of the circulating pump is connected with the hydraulic micro-interface generator.
Preferably, the top of the mixing tank is connected with a catalyst pipeline, and the side wall of the mixing tank is connected with a succinic acid pipeline and a 1, 4-butanediol pipeline.
Preferably, the outer side of the esterification reactor is connected with a heat exchanger for ensuring the temperature of the esterification reaction.
In addition, the invention also provides a micro-interface method for preparing the polybutylene succinate, which comprises the following steps:
premixing 1, 4-butanediol, succinic acid and a proper amount of catalyst, and then carrying out esterification reaction, rectification and vacuum polycondensation to obtain a poly (butylene succinate) product.
Preferably, the temperature of the esterification reaction is 130-170 ℃.
Preferably, the temperature of the vacuum polycondensation is 200-240 ℃, and the pressure is 0.005-0.05 MPa.
Compared with the prior art, the invention has the advantages that:
(1) through the inside at esterification reactor is provided with linkage micro-interface generator, with succinic acid, 1, 4 butanediol and catalyst dispersion breakage, can make succinic acid, 1, 4 butanediol and catalyst mutually dissolve better like this, solution temperature, concentration distribution are more even, have greatly strengthened the torrent degree of solution moreover for solid-liquid phase boundary layer further thins, increases substantially reaction efficiency, has practiced thrift manufacturing cost, improves production efficiency and output ratio.
(2) The hydraulic micro-interface generator can make the material have a certain flow velocity, and the catalyst can be dispersed to each part of the esterification reactor, so that the reaction rate is obviously improved.
Drawings
Various other advantages and benefits will become apparent to those of ordinary skill in the art upon reading the following detailed description of the preferred embodiments. The drawings are only for purposes of illustrating the preferred embodiments and are not to be construed as limiting the invention. Also, like reference numerals are used to refer to like parts throughout the drawings. In the drawings:
FIG. 1 is a schematic structural diagram of a micro-interface system for preparing polybutylene succinate provided by the invention;
wherein:
10-a mixing tank; 11-a catalyst conduit;
12-a succinic acid conduit; a 13-1, 4 butanediol line;
20-an esterification reactor; 21-a linkage type micro-interface generator;
211-a hydrodynamic micro-interface generator; 212-a pneumatic micro-interface generator;
213-connecting the pipeline; 22-a heat exchanger;
23-a circulation pump; 231-pump outlet;
30-a rectifying tower; 40-vacuum polycondensation tower.
Detailed Description
The technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings and the detailed description, but those skilled in the art will understand that the following described embodiments are some, not all, of the embodiments of the present invention, and are only used for illustrating the present invention, and should not be construed as limiting the scope of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc., indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
In order to more clearly illustrate the technical solution of the present invention, the following description is made in the form of specific embodiments.
Example 1
Referring to fig. 1, a schematic structural diagram of a micro-interface system for preparing polybutylene succinate according to the present invention includes a mixing tank 10, in which the mixing tank 10 mixes a catalyst from a catalyst pipeline 11 at the top, succinic acid from a succinic acid pipeline 12 at the side wall, and 1, 4-butanediol from a 1, 4-butanediol pipeline 13, and then sends the mixture to an esterification reactor 20. The esterification reactor 20 is internally provided with a linkage type micro-interface generator 21, and the linkage type micro-interface generator 21 mainly comprises a hydraulic type micro-interface generator 211, a pneumatic type micro-interface generator 212 and a communicating pipeline 213. The hydraulic micro-interface generator 211 is arranged right above the pneumatic micro-interface generator 212, and the hydraulic micro-interface generator 211 is connected with the pneumatic micro-interface generator 212 through a communication pipeline 213. The hydraulic micro-interface generator 211 is connected with a circulating pump 23, and the circulating pump 23 pumps and pressurizes the material in the middle of the esterification reactor 20 and returns the material to the hydraulic micro-interface generator 211.
A heat exchanger 22 is also connected to the exterior of the esterification reactor 20 to ensure that the temperature of the esterification reaction is maintained between 170 ℃. Then the material enters a rectifying tower 30 for distillation, when the water yield of distilled water is 95 percent of the theoretical water yield, the material is conveyed to a vacuum polycondensation tower 40, the vacuum polycondensation tower 40 is vacuumized to 0.05MPa, and the temperature is maintained at 200 ℃. And finally, cooling. And slicing to obtain a finished product of the poly (butylene succinate).
The reaction process comprises the steps of premixing 1, 4-butanediol, succinic acid and a proper amount of catalyst, and then carrying out esterification reaction, rectification and vacuum polycondensation to obtain a poly (butylene succinate) product. The temperature of the esterification reaction was 130 ℃. The temperature of the vacuum polycondensation is 200 ℃ and the pressure is 0.05 MPa. .
Example 2
The other operating steps are identical to those of example 1, except that: the linkage type micro-interface generator consists of two pneumatic type micro-interface generators. At this time, the temperature of the esterification reaction was 170 ℃ and the temperature of the vacuum polycondensation was 240 ℃ and the pressure was 0.005 MPa.
Example 3
The other operating steps are identical to those of example 1, except that: the hydraulic micro-interface generator and the pneumatic micro-interface generator are horizontally arranged.
Comparative example 1
The other operating steps are identical to those of example 1, except that: the esterification reactor is not provided with a linkage type micro-interface generator.
| Temperature (. degree.C.) for esterification reaction | Weight average molecular weight (g/mol) | |
| Example 1 | 130 | 90000 |
| Example 2 | 140 | 57100 |
| Example 3 | 170 | 52400 |
| Comparative example 1 | 110 | 45000 |
According to the data, the conclusion can be drawn that the linkage type micro-interface generator is adopted, and the linkage type micro-interface generator can achieve the optimal effect by adopting a hydraulic type micro-interface generator and a pneumatic type micro-interface generator.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. The utility model provides a preparation olybuthylenesuccinate's micro-interface system which characterized in that, includes and is used for mixing tank premixed with succinic acid, 1, 4 butanediol and catalyst, the mixing tank is connected with the esterification reaction ware, the inside of esterification reaction ware is provided with linkage formula micro-interface generator, linkage formula micro-interface generator is connected with the circulating pump, esterification reaction ware has connected gradually rectifying column and vacuum polycondensation tower afterwards.
2. The micro-interface system of claim 1, wherein the ganged micro-interface generator comprises a hydraulic micro-interface generator and a pneumatic micro-interface generator.
3. The micro-interface system of claim 2, wherein the hydrodynamic micro-interface generator is disposed directly above the pneumatic micro-interface generator.
4. The micro-interface system of claim 2, further comprising a communication conduit connecting the hydrodynamic micro-interface generator and the pneumatic micro-interface generator.
5. The micro-interface system of claim 2, wherein the outlet of the circulating pump is connected to the hydrodynamic micro-interface generator.
6. The micro-interface system of claim 1, wherein a catalyst line is connected to the top of the mixing tank, and a succinic acid line and a 1, 4-butanediol line are connected to the side wall of the mixing tank.
7. The micro-interface system of claim 1, wherein a heat exchanger is connected to the outside of the esterification reactor to ensure the temperature of the esterification reaction.
8. A method for preparing a poly (butylene succinate) micro-interface system according to any one of claims 1 to 7, comprising the following steps:
premixing 1, 4-butanediol, succinic acid and a proper amount of catalyst, and then carrying out esterification reaction, rectification and vacuum polycondensation to obtain a poly (butylene succinate) product.
9. The micro-interface system of claim 8, wherein the esterification reaction temperature is 130-170 ℃.
10. The micro-interface system as claimed in claim 8, wherein the temperature of the vacuum polycondensation is 200 ℃ and 240 ℃, and the pressure is 0.005-0.05 MPa.
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2022
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| CN102597054A (en) * | 2009-10-21 | 2012-07-18 | 株式会社日立工业设备技术 | Device and method for producing polybutylene succinate |
| CN112521250A (en) * | 2020-11-30 | 2021-03-19 | 南京延长反应技术研究院有限公司 | Micro-interface reaction system and method for preparing ethylene glycol by gas-phase catalytic hydration method |
| CN112794996A (en) * | 2020-12-29 | 2021-05-14 | 中国纺织科学研究院有限公司 | Preparation system and preparation method of biodegradable copolyester and copolyester thereof |
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