CN110078903A - A method of continuously preparing Biodegradable resin side by side - Google Patents
A method of continuously preparing Biodegradable resin side by side Download PDFInfo
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- CN110078903A CN110078903A CN201910415295.1A CN201910415295A CN110078903A CN 110078903 A CN110078903 A CN 110078903A CN 201910415295 A CN201910415295 A CN 201910415295A CN 110078903 A CN110078903 A CN 110078903A
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- 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
- C08G63/18—Dicarboxylic acids and dihydroxy compounds the acids or hydroxy compounds containing carbocyclic rings
- C08G63/181—Acids containing aromatic rings
- C08G63/183—Terephthalic acids
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- 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
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polyesters Or Polycarbonates (AREA)
Abstract
The invention discloses a kind of methods for continuously preparing Biodegradable resin side by side, specific steps are as follows: first independently configure slurry A and slurry B；Slurry A and slurry B in step 1 are added continuously to carry out esterification in the esterifier of respective unit respectively, and two kinds of carboxylates are respectively prepared；2 kinds of carboxylates that step 2 obtains are continuously fed to mixing esterifier and carry out mixing esterification, obtain mixed ester compound；The mixed ester compound that step 3 obtains is continuously fed to Prepolycondensating reactor and carries out preliminary polycondensation reaction；The prepolymer that step 4 obtains is continuously fed in final polycondensation reactor, carries out interim polycondensation reaction；The polymer for the higher molecular weight that step 5 obtains is continuously fed to carry out further polymerization reaction in a viscosity-increasing reactor.The method that block form of the invention continuously prepares Biodegradable resin can obtain multiple kinds, and product is versatile and flexible, meet the demand of the needs of turn of the market and national development.
Description
Technical field
A kind of preparing the present invention relates to polymerization macromolecule resin technical field more particularly to continuously Biodegradable resin side by side
Method.
Background technique
With the development of science and technology the raising of living standards of the people, high molecular material especially synthesize macromolecule, such as plastics, tree
The status in people's lives such as rouge is more and more important, and widened trend year by year is also presented in application.Global plastics, synthetic resin
Etc. the synthesis high molecular materials of classes have become the third-largest important materials for being only second to metal and cement.But since plastics etc. are general
Type high molecular material class product is all the derivative of oil product, belongs to hydrocarbon organic matter, is difficult to decompose in its natural state,
Its waste has become the source of " white pollution ", become seriously affect environment and human kind sustainable development social concern it
One.
For environment purification, the synthesis waste polymer material such as plastics is eliminated, synthesis and degradation high molecular material is just at drop
The mainstream of resin material exploitation is solved, wherein aliphatic polyester is due to its excellent physical property, degradation property and suitable cost
Become the emphasis of current degradative plastics exploitation.
In order to realize that these high performance materials break the monopolization of foreign technology company, the present invention proposes a kind of system continuous side by side
The method of standby Biodegradable resin, the poly terephthalic acid-tetramethylene adipate or poly terephthalic acid-succinic acid produced
Butanediol ester belongs to one kind of third generation biological degradation plastics aliphatic dibasic acid glycol polyesters, it has excellent toughness
And heat resistance, processing performance is good, and price is relatively low, and general-purpose plastics level is fully achieved in its performance.And as raw material
Can be used for making the disposable products such as packaging material, table ware, amenities and mulch, and be expected medical material,
The high-tech sectors such as photoelectron chemistry, fine chemistry industry are used widely, and have broad mass market prospect.
Summary of the invention
The purpose of the present invention is to solve the problems of the prior art, and a kind of preparation biology drop continuous side by side proposed
The method for solving resin.
To achieve the goals above, present invention employs following technical solutions:
A method of Biodegradable resin continuously being prepared side by side, specific steps are as follows:
S1: slurry A and slurry B is first independently configured；
S2: slurry A and slurry B in step 1 are added continuously to be esterified in the esterifier of respective unit respectively
Reaction, is respectively prepared two kinds of carboxylates；
S3: 2 kinds of carboxylates that step 2 obtains are continuously fed to mixing esterifier and carry out mixing esterification, obtain
Mixed ester compound；
S4: the mixed ester compound that step 3 obtains is continuously fed to Prepolycondensating reactor and carries out preliminary polycondensation reaction, reactor
Interior pressure requirements are 500Pa-5000Pa, carry out polycondensation reaction with this condition and obtain prepolymer；
S5: the prepolymer that step 4 obtains is continuously fed in final polycondensation reactor, carries out interim polycondensation reaction, instead
Answering pressure requirements in device is 100pa-500pa, carries out polycondensation reaction with this condition and obtains the higher polymer of molecular weight；
S6: the polymer for the higher molecular weight that step 5 obtains is continuously fed to carry out in a viscosity-increasing reactor further
Polymerization reaction, reactor pressure require to be 50pa-200pa, obtain molecular weight very carrying out polycondensation reaction with this condition
High polymer；
S7: the heavy polymer, which passes through, to be granulated, is dry, being packaged to be Biodegradable resin slice.
Preferably, the raw material of slurry A and slurry B are binary acid and dihydric alcohol, the slurry A raw material in the step 1
Binary acid be terephthalic acid (TPA), dihydric alcohol is 1,4-butanediol, and alkyd is in molar ratio: 1.0-2.0 carry out step 2 in
Esterification, and into catalyst required for addition before esterifier in step 2；
The binary acid of the slurry B raw material is Isosorbide-5-Nitrae fourth dioctyl phthalate or 1, and the own dioctyl phthalate of 6-, dihydric alcohol is Isosorbide-5-Nitrae-fourth two
Alcohol, alkyd in molar ratio: 1.0-2.0 carry out step 2 in esterification.
Preferably, step 2 terephthalic acid (TPA) and 1,4-butanediol esterification reaction temperature are 190-240 DEG C, reaction pressure
Power is absolute pressure 60-100Pa, and residence time 1.5-4 hour, the control of reactor esterification yield is 90% or more out；
And to Isosorbide-5-Nitrae fourth dioctyl phthalate or 1, the own dioctyl phthalate of 6- and 1,4-butanediol esterification reaction temperature are 140-220 DEG C, reaction
Pressure is absolute pressure 60-100Pa, and residence time 1.5-4 hour, the control of reactor esterification yield is 92% or more out.
Preferably, the step 3 is mixing in esterifier,
Reaction condition are as follows: 190-240 DEG C of reaction temperature, reaction pressure is absolute pressure 10-70Pa, residence time 1.0-3 hour；
And two kinds of carboxylate mass ratios: 0.5-1.5.
Preferably, the step 4 is in Prepolycondensating reactor,
Reaction condition are as follows: 200-250 DEG C of reaction temperature, reaction pressure is absolute pressure 0.5-5KPa, and the residence time, 0.5-3 was small
When；
Catalyst, heat stabilizer, antioxidant required for polycondensation are being added into before Prepolycondensating reactor.
Preferably, the step 5 is in final polycondensation reactor,
Reaction condition are as follows: 220-270 DEG C of reaction temperature, reaction pressure is absolute pressure 100-500Pa, and the residence time, 1.5-4 was small
When；
Catalyst, modifying agent required for polycondensation are being added into before final polycondensation reactor.
Preferably, the step 6 is in viscosity-increasing reactor,
Reaction condition are as follows: 230-280 DEG C of reaction temperature, reaction pressure is absolute pressure 50-200Pa, and the residence time, 1.5-3 was small
When；
Chain extender, modifying agent required for polycondensation are being added into before final polycondensation reactor.
Compared with prior art, the present invention provides it is a kind of side by side continuously prepare Biodegradable resin method, have with
It is lower the utility model has the advantages that
Entitled poly terephthalic acid-the tetramethylene adipate of obtained polymer chemistry or poly terephthalic acid-fourth
Succinate adipate, and the melt index of Biodegradable resin, less than 6, product can be widely applied to engineering plastics, fibre
The fields such as dimension, film, the method that block form continuously prepares Biodegradable resin can obtain multiple kinds, and product is versatile and flexible,
Meet the demand of the needs of turn of the market and national development, builds " innovation-oriented country " and " energy-saving and emission-reduction, establishing resource saving
The development strategy of type, friendly environment society " has significant environmental benefit and social benefit, while having good economy
Benefit.
It is not directed to part in the invention to be the same as those in the prior art or can be realized by using the prior art, structure of the invention
Simply, easy to operate.
Detailed description of the invention
Fig. 1 is a kind of flow chart of method for continuously preparing Biodegradable resin side by side proposed by the present invention.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.
Embodiment 1
As shown in Figure 1, a kind of method for continuously preparing Biodegradable resin side by side, by terephthalic acid (TPA) (PTA) and Isosorbide-5-Nitrae-
1:1.6 is modulated into slurry to butanediol in molar ratio in 1 slurry tank, is sent to the flow of 681kg/H to 1 by delivery pump
It is esterified in esterifier, at 235 DEG C, pressure is controlled in absolute pressure 75kPa for esterification temperature control, is continuously added in esterification
0.2kg butyl titanate carries out esterification rate and reaches 92% or more；
In addition, by adipic acid and 1,4-butanediol, 1:1.4 is modulated into slurry in molar ratio in 2 slurry tanks simultaneously, pass through
Delivery pump is sent into 2 esterifiers with the flow of 745kg/H and is esterified, and esterification temperature control is at 180 DEG C, pressure
Control carries out esterification rate and reaches 95% or more in absolute pressure 85kPa,
The carboxylate in 1 esterifier and in 2 esterifiers is proportionally sent to mixed ester by delivery pump
Change in reactor, mixes the temperature control in esterifier at 238 DEG C, pressure is controlled in absolute pressure 65kPa, continues to be esterified
Reaction, esterification rate reach 96% or more；
It is sent in Prepolycondensating reactor by delivery pump later, at 235 DEG C, pressure control exists for the temperature control of reactor
Antimony oxide 0.28kg/H is added under this condition, is sent to final minification by delivery pump after stop 60min and gathers instead by absolute pressure 1kPa
It answers in device；
Temperature control in final polycondensation reactor at 242 DEG C, pressure control in absolute pressure 200Pa, under the conditions of reacted
After stopping 120min, melt is sent in viscosity-increasing reactor by delivery pump, the temperature in viscosity-increasing reactor is controlled 242
DEG C, pressure control in absolute pressure 100Pa, under the conditions of reacted, after the viscosity of material reaches 1200Pa.S, passing through delivery pump will
Melt is sent to pelletizing and is granulated, dried, packed, high polymer melt poly terephthalic acid-tetramethylene adipate of acquisition；
It is 190 DEG C, 2.16kg in test condition, the melt index of melt is 4.
Embodiment 2
As shown in Figure 1, a kind of method for continuously preparing Biodegradable resin side by side, by terephthalic acid (TPA) (PTA) and Isosorbide-5-Nitrae-
1:1.6 is modulated into slurry to butanediol in molar ratio in 1 slurry tank, is sent to the flow of 650kg/H to 1 by delivery pump
It is esterified in esterifier, at 235 DEG C, pressure is controlled in absolute pressure 75kPa for esterification temperature control, is continuously added in esterification
0.2kg butyl titanate carries out esterification rate and reaches 92% or more；
In addition, by succinic acid and 1,4-butanediol, 1:1.6 is modulated into slurry in molar ratio in 2 slurry tanks simultaneously, pass through
Delivery pump is sent into 2 esterifiers with the flow of 800kg/H and is esterified, and esterification temperature control is at 145 DEG C, pressure
Control carries out esterification rate and reaches 92% or more in absolute pressure 70kPa；
The carboxylate in 1 esterifier and in 2 esterifiers is proportionally sent to mixed ester by delivery pump
Change in reactor, mixes the temperature control in esterifier at 238 DEG C, pressure is controlled in absolute pressure 65kPa, continues to be esterified
Reaction, esterification rate reach 96% or more；
It is sent in Prepolycondensating reactor by delivery pump later, at 240 DEG C, pressure control exists for the temperature control of reactor
Antimony oxide 0.285kg/H is added under this condition, is sent to final minification by delivery pump after stop 90min and gathers by absolute pressure 1kPa
In reactor；
Temperature control in final polycondensation reactor at 242 DEG C, pressure control in absolute pressure 200Pa, under the conditions of reacted
After stopping 140min, melt is sent in viscosity-increasing reactor by delivery pump, the temperature in viscosity-increasing reactor is controlled 242
DEG C, pressure control in absolute pressure 50Pa, under the conditions of carry out reaction 60min, after the viscosity of material reaches 1300Pa.S, pass through conveying
Melt is sent to pelletizing and is granulated, dries, packs, high polymer melt poly terephthalic acid-succinic acid fourth two of acquisition by pump
Alcohol ester；
It is 190 DEG C, 2.16kg in test condition, the melt index of melt is 5.
Embodiment 3
As shown in Figure 1, a kind of method for continuously preparing Biodegradable resin side by side, by fourth dioctyl phthalate (SA) and Isosorbide-5-Nitrae-fourth two
1:1.6 is modulated into slurry to alcohol in molar ratio in 1 slurry tank, is sent to the flow of 1000kg/H to 1 ester by delivery pump
Change and be esterified in reactor, at 145 DEG C, pressure is controlled in absolute pressure 75kPa for esterification temperature control, is continuously added in esterification
0.2kg butyl titanate carries out esterification rate and reaches 92% or more；
In addition, by adipic acid and 1,4-butanediol, 1:1.4 is modulated into slurry in molar ratio in 2 slurry tanks simultaneously, pass through
Delivery pump is sent into 2 esterifiers with the flow of 350kg/H and is esterified, and esterification temperature control is at 180 DEG C, pressure
Control carries out esterification rate and reaches 95% or more in absolute pressure 85kPa；
The carboxylate of 1 esterifier and 2 esterifiers is proportionally sent to mixing esterification instead by delivery pump
It answers in device, mixes the temperature control in esterifier at 190 DEG C, it is anti-to continue esterification in absolute pressure 60kPa for pressure control
It answers, esterification rate reaches 96% or more；
It is sent in Prepolycondensating reactor by delivery pump later, at 235 DEG C, pressure control exists for the temperature control of reactor
Absolute pressure 800kPa.Antimony oxide 0.28kg/H is added under this condition, final minification is sent to by delivery pump after stop 75min and is gathered
In reactor.Temperature control in final polycondensation reactor at 240 DEG C, pressure control in absolute pressure 200Pa, under the conditions of reacted
After stopping 120min, melt is sent in viscosity-increasing reactor by delivery pump, the temperature in viscosity-increasing reactor is controlled 236
DEG C, pressure control in absolute pressure 40Pa, under the conditions of reacted, after the viscosity of material reaches 1200Pa.S, passing through delivery pump will
Melt is sent to pelletizing and is granulated, dried, packed, high polymer melt polybutadiene formic acid-tetramethylene adipate of acquisition；
It is 190 DEG C, 2.16kg in test condition, the melt index of melt is 6.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (7)
1. it is a kind of side by side continuously prepare Biodegradable resin method, which is characterized in that it is described specific steps are as follows:
S1: slurry A and slurry B is first independently configured；
S2: slurry A and slurry B in step (1) are added continuously to carry out being esterified in the esterifier of respective unit respectively anti-
It answers, two kinds of carboxylates is respectively prepared；
S3: 2 kinds of carboxylates that step (2) obtains are continuously fed to mixing esterifier and carry out mixing esterification, are mixed
Close carboxylate；
S4: the mixed ester compound that step (3) obtains is continuously fed to Prepolycondensating reactor and carries out preliminary polycondensation reaction, in reactor
Pressure requirements are 500Pa-5000Pa, carry out polycondensation reaction with this condition and obtain prepolymer；
S5: the prepolymer that step (4) obtains is continuously fed in final polycondensation reactor, carries out interim polycondensation reaction, reaction
Pressure requirements are 100pa-500pa in device, carry out polycondensation reaction with this condition and obtain the higher polymer of molecular weight；
S6: the polymer for the higher molecular weight that step (5) obtains is continuously fed to further be gathered in a viscosity-increasing reactor
Reaction is closed, reactor pressure requires to be 50pa-200pa, and it is very high to obtain molecular weight for progress polycondensation reaction with this condition
Polymer；
S7: the heavy polymer, which passes through, to be granulated, is dry, being packaged to be Biodegradable resin slice.
2. a kind of method for continuously preparing Biodegradable resin side by side according to claim 1, which is characterized in that the step
Suddenly the raw material of slurry A and slurry B are binary acid and dihydric alcohol in (1), and the binary acid of the slurry A raw material is terephthaldehyde
Acid, dihydric alcohol is 1,4-butanediol, and alkyd is in molar ratio: 1.0-2.0 carries out the esterification in step (2), and walks
Suddenly into catalyst required for addition before esterifier in (2)；
The binary acid of the slurry B raw material is Isosorbide-5-Nitrae fourth dioctyl phthalate or 1, and the own dioctyl phthalate of 6-, dihydric alcohol is 1,4-butanediol, alcohol
Acid in molar ratio: 1.0-2.0 carry out step (2) in esterification.
3. a kind of method for continuously preparing Biodegradable resin side by side according to claim 1, which is characterized in that the step
Suddenly (2) terephthalic acid (TPA) and 1,4-butanediol esterification reaction temperature are 190-240 DEG C, and reaction pressure is absolute pressure 60-100Pa, are stopped
Time 1.5-4 hour is stayed, the control of reactor esterification yield is 90% or more out；
And to Isosorbide-5-Nitrae fourth dioctyl phthalate or 1, the own dioctyl phthalate of 6- and 1,4-butanediol esterification reaction temperature are 140-220 DEG C, reaction pressure
For absolute pressure 60-100Pa, residence time 1.5-4 hour, the control of reactor esterification yield is 92% or more out.
4. a kind of method for continuously preparing Biodegradable resin side by side according to claim 1, which is characterized in that the step
Suddenly (3) are mixing in esterifier,
Reaction condition are as follows: 190-240 DEG C of reaction temperature, reaction pressure is absolute pressure 10-70Pa, residence time 1.0-3 hour；
And two kinds of carboxylate mass ratios: 0.5-1.5.
5. a kind of method for continuously preparing Biodegradable resin side by side according to claim 1, which is characterized in that the step
Suddenly (4) in Prepolycondensating reactor,
Reaction condition are as follows: 200-250 DEG C of reaction temperature, reaction pressure is absolute pressure 0.5-5KPa, residence time 0.5-3 hour；
Catalyst, heat stabilizer, antioxidant required for polycondensation are being added into before Prepolycondensating reactor.
6. a kind of method for continuously preparing Biodegradable resin side by side according to claim 1, which is characterized in that the step
Suddenly (5) in final polycondensation reactor,
Reaction condition are as follows: 220-270 DEG C of reaction temperature, reaction pressure is absolute pressure 100-500Pa, residence time 1.5-4 hour；
Catalyst, modifying agent required for polycondensation are being added into before final polycondensation reactor.
7. a kind of method for continuously preparing Biodegradable resin side by side according to claim 1, which is characterized in that the step
Suddenly (6) in viscosity-increasing reactor,
Reaction condition are as follows: 230-280 DEG C of reaction temperature, reaction pressure is absolute pressure 50-200Pa, residence time 1.5-3 hour；
Chain extender, modifying agent required for polycondensation are being added into before final polycondensation reactor.
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| CN201910415295.1A CN110078903A (en) | 2019-05-17 | 2019-05-17 | A method of continuously preparing Biodegradable resin side by side |
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Cited By (6)
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|---|---|---|---|---|
| CN111363131A (en) * | 2020-03-19 | 2020-07-03 | 戴清文 | Biodegradable aliphatic-aromatic copolyester with low carboxyl content and continuous preparation method thereof |
| CN111440301A (en) * | 2020-05-06 | 2020-07-24 | 扬州惠通化工科技股份有限公司 | Multifunctional polyester continuous production system |
| CN112898546A (en) * | 2021-03-24 | 2021-06-04 | 山东道恩高分子材料股份有限公司 | Preparation method of PBAT material with high thermal stability |
| CN113234213A (en) * | 2021-04-21 | 2021-08-10 | 中国纺织科学研究院有限公司 | PBST polymer, preparation method and application thereof, and agricultural mulching film |
| CN113234212A (en) * | 2021-03-31 | 2021-08-10 | 山东道恩高分子材料股份有限公司 | Method and device for continuously preparing high-quality PBAT |
| WO2021244193A1 (en) * | 2020-06-01 | 2021-12-09 | 欧瑞康巴马格惠通（扬州）工程有限公司 | System for producing pbs-based biodegradable material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111363131A (en) * | 2020-03-19 | 2020-07-03 | 戴清文 | Biodegradable aliphatic-aromatic copolyester with low carboxyl content and continuous preparation method thereof |
| CN111363131B (en) * | 2020-03-19 | 2022-06-10 | 戴清文 | Biodegradable aliphatic-aromatic copolyester with low carboxyl content and continuous preparation method thereof |
| CN111440301A (en) * | 2020-05-06 | 2020-07-24 | 扬州惠通化工科技股份有限公司 | Multifunctional polyester continuous production system |
| CN111440301B (en) * | 2020-05-06 | 2023-10-31 | 扬州惠通科技股份有限公司 | Multifunctional polyester continuous production system |
| WO2021244193A1 (en) * | 2020-06-01 | 2021-12-09 | 欧瑞康巴马格惠通（扬州）工程有限公司 | System for producing pbs-based biodegradable material |
| CN112898546A (en) * | 2021-03-24 | 2021-06-04 | 山东道恩高分子材料股份有限公司 | Preparation method of PBAT material with high thermal stability |
| CN113234212A (en) * | 2021-03-31 | 2021-08-10 | 山东道恩高分子材料股份有限公司 | Method and device for continuously preparing high-quality PBAT |
| CN113234213A (en) * | 2021-04-21 | 2021-08-10 | 中国纺织科学研究院有限公司 | PBST polymer, preparation method and application thereof, and agricultural mulching film |
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