CN203938629U - The production unit of poly butylene succinate - Google Patents
The production unit of poly butylene succinate Download PDFInfo
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- CN203938629U CN203938629U CN201420404696.XU CN201420404696U CN203938629U CN 203938629 U CN203938629 U CN 203938629U CN 201420404696 U CN201420404696 U CN 201420404696U CN 203938629 U CN203938629 U CN 203938629U
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Abstract
The utility model relates to the production unit of poly butylene succinate, and it comprises: by pipeline successively connected slurry modulation tank, the first esterifying kettle, second esterification kettle, precondensation still, whole polycondensation vessel, viscosity-increasing reactor; The first esterifying kettle, second esterification kettle are respectively equipped with esterification steam outlet, two esterification steam outlets are all connected with the isolate entrance of knockout tower by pipeline, and the heavy constituent outlet of knockout tower is connected with the component regenerant entrance of the first esterifying kettle, second esterification kettle by pipeline; On the pipeline between second esterification kettle and precondensation still, be provided with transferpump and oligopolymer well heater; On the pipeline between precondensation still and whole polycondensation vessel, properties-correcting agent adder and static mixer are set; Viscosity-increasing reactor is provided with melt outlet, and melt outlet is connected by melt pipe with the melt inlet of fondant filter.The utility model can improve viscosity and the productive rate of poly butylene succinate.
Description
Technical field
The utility model relates to Chemicals production unit field, in particular to the production unit of poly butylene succinate.
Background technology
Poly butylene succinate, English full name is Poly (butylene succinate), is called for short PBS, is a kind of Biodegradable polymer material.First, PBS kind polyester has good over-all properties, and not only mechanical property can meet the service requirements of general-purpose plastics, and its just degraded under the condition of the contact microorganisms such as compost, highly stable in normal storage and use procedure performance.The second, PBS processing characteristics is very good, can on general processing units, carry out all kinds of forming process, is processing characteristics best (this point is most important to degradative plastics application) in current universal degradative plastics.The 3rd, PBS series polyester has outstanding resistance toheat, and heat-drawn wire approaches 100 ℃, after modification, can surpass 100 ℃ (resistance toheat is best in totally biodegradable polyester), meet the heat-resisting demand of articles for daily use, can be used for preparing cold and hot drink packing and cutlery box.Meanwhile, PBS kind polyester has price advantage, and after scale production, price can reach the level of PET polyester.
By succinic acid and 1,4-butyleneglycol is directly synthetic can access PBS, its synthesis technique is, first in esterifying kettle, carry out the diprotic acid of lower temperature of reaction and excessive dibasic alcohol ester, then carboxylate enters precondensation still, removes small molecules and forms hydroxyl terminated prepolymer, then at material, enters whole polycondensation vessel, under the existence of high temperature, high vacuum and catalyzer, remove dibasic alcohol, obtain PBS.But adopt the productive rate of PBS prepared by this production unit lower, viscosity is not high.
Utility model content
The purpose of this utility model is to provide a kind of production unit of poly butylene succinate, lower to solve the PBS productive rate obtaining in existing direct esterification reaction, the problem that viscosity is not high.
The utility model embodiment provides a kind of production unit of poly butylene succinate, comprising: by pipeline successively connected slurry modulation tank, the first esterifying kettle, second esterification kettle, precondensation still, whole polycondensation vessel, viscosity-increasing reactor; Wherein,
Described slurry modulation tank is connected with succinic acid squirt pump, BDO transport pipe, catalyzer duct respectively;
Described the first esterifying kettle, described second esterification kettle are respectively equipped with esterification steam outlet, two described esterification steam outlets are all connected with the isolate entrance of knockout tower by pipeline, and the heavy constituent outlet of described knockout tower is connected with the component regenerant entrance of described the first esterifying kettle, described second esterification kettle by pipeline;
On the pipeline between described second esterification kettle and described precondensation still, be provided with transferpump and oligopolymer well heater;
On the pipeline between described precondensation still and described whole polycondensation vessel, properties-correcting agent adder and static mixer are set;
Described precondensation still, described whole polycondensation vessel, described viscosity-increasing reactor are connected with vacuum system by gas phase pipeline respectively, on described gas phase pipeline, condensing works are set;
Described viscosity-increasing reactor is provided with melt outlet, and described melt outlet is connected by melt pipe with the melt inlet of fondant filter.
In certain embodiments, be preferably, described properties-correcting agent adder is syringe or squirt pump.
In certain embodiments, be preferably, on described melt pipe, static mixer be set.
In certain embodiments, be preferably, the production unit of described poly butylene succinate also comprises dicing machine, and described dicing machine is connected with described fondant filter.
In certain embodiments, be preferably, described condensing works is spray condenser, and low temperature BDO is housed in described spray condenser.
In certain embodiments, be preferably, described the first esterifying kettle, described second esterification kettle, described precondensation still, described whole polycondensation vessel, described viscosity-increasing reactor are equipped with well heater.
In certain embodiments, be preferably, described well heater is gas heat conducting oil stove.The light constituent outlet of described knockout tower and the regenerant entrance of tetrahydrofuran (THF) recovery system
In certain embodiments, be preferably, the light constituent outlet of described knockout tower is connected by pipeline with the regenerant entrance of tetrahydrofuran (THF) recovery system.
The production unit of the poly butylene succinate that the utility model embodiment provides, compared with prior art, native system has carried out thinner division by esterification and polycondensation reactor, esterification is respectively at the first esterifying kettle, in second esterification kettle, carry out successively, product after esterification can enter precondensation still successively, whole polycondensation vessel, viscosity-increasing reactor, wherein viscosity-increasing reactor is exactly a kind of polycondensation vessel of tackify in fact, material carries out differing temps in different reactors, different vacuum tightness, the reaction of differential responses time, remove small molecules, temperature, vacuum tightness increases gradually, improved the viscosity productive rate of final product PBS.
Accompanying drawing explanation
Fig. 1 is the connection diagram of each equipment in poly butylene succinate production unit in embodiment of the utility model.
Embodiment
Below by specific embodiment, by reference to the accompanying drawings the utility model is described in further detail.
Consider that in current direct esterification, poly butylene succinate viscosity is low, the problem that productive rate is low, provides a kind of production unit of poly butylene succinate at the utility model embodiment.
The production unit of this poly butylene succinate, comprising: by pipeline successively connected slurry modulation tank, the first esterifying kettle, second esterification kettle, precondensation still, whole polycondensation vessel, viscosity-increasing reactor; Wherein,
Described slurry modulation tank is connected with succinic acid squirt pump, BDO transport pipe, catalyzer duct respectively;
Described the first esterifying kettle, described second esterification kettle are respectively equipped with esterification steam outlet, two described esterification steam outlets are all connected with the isolate entrance of knockout tower by pipeline, and the heavy constituent outlet of described knockout tower is connected with the component regenerant entrance of described the first esterifying kettle, described second esterification kettle by pipeline;
On the pipeline between described second esterification kettle and described precondensation still, be provided with transferpump and oligopolymer well heater;
On the pipeline between described precondensation still and described whole polycondensation vessel, properties-correcting agent adder and static mixer are set;
Described precondensation still, described whole polycondensation vessel, described viscosity-increasing reactor are connected with vacuum system by gas phase pipeline respectively, on described gas phase pipeline, condensing works are set;
Described viscosity-increasing reactor is provided with melt outlet, and described melt outlet is connected by melt pipe with the melt inlet of fondant filter.
Native system has carried out thinner division by esterification and polycondensation reactor, esterification is carried out successively respectively in the first esterifying kettle, second esterification kettle, product after esterification can enter precondensation still, whole polycondensation vessel, viscosity-increasing reactor successively, wherein viscosity-increasing reactor is exactly a kind of polycondensation vessel of tackify in fact, material carries out differing temps, different vacuum tightness, the reaction of differential responses time in different reactors, remove small molecules, temperature, vacuum tightness increase gradually, have improved the viscosity productive rate of final product PBS.
Next the production unit of this poly butylene succinate is made a more detailed description, as shown in Figure 1:
Succinic acid self-injection pump sprays into slurry modulation tank D01,1,4-butyleneglycol is from 1,4-butyleneglycol transport pipe is sent into slurry modulation tank D01, catalyzer autocatalysis agent delivery tube is sent into slurry modulation tank D01, through fully dissolving, stirring, be evenly mixed with into mixed slurry, slurries filtration is delivered to the first esterifying kettle D02 by transferpump; Mixed slurry at 160～170 ℃, carries out the first esterification at the first esterifying kettle D02 under 80kPaA condition, under this temperature of reaction, pressure, control esterification yield, and this esterification yield reaches more than 96%.Then, the carboxylate obtaining in the first esterifying kettle D02 is sent in second esterification kettle D03, and it is 170～180 ℃ that temperature of reaction is controlled, and reaction pressure is controlled as 80kPaA, and esterification yield reaches more than 98.5%, the first esterifying kettle D02, the water that second esterification kettle D03 generates and 1, the tetrahydrofuran (THF) (THF) that 4-butyleneglycol (BDO) cyclization generates and the BDO taking out of and carboxylate etc. form esterification steam, this esterification steam enters knockout tower D07 and carries out separation, at the bottom of tower, heavy constituent is returned to the first esterifying kettle D02, second esterification kettle D03, water and the THF steam that discharges at knockout tower D07 top enter esterification water return tank after condensation, THF and water mixture can be sent into (the light constituent outlet (water and THF steam) of knockout tower D07 is connected by pipeline with the regenerant entrance of THF recovery system) in THF recovery system.Subsequently, the oligopolymer that second esterification kettle D03 reaction obtains is sent into precondensation still D04 through transferpump by oligopolymer well heater, precondensation makes the small molecules that polycondensation is deviate from constantly shift out under heat-conducting oil heating and high vacuum condition, impels polycondensation to think that positive reaction direction carries out.The temperature of this prepolymerization reaction is controlled at 230～240 ℃, and reaction pressure is controlled at 2～4kPaA, and the residence time is controlled at 2.5 hours.Under the parameter in this temperature, pressure, reaction times is controlled, when touching the mark, the polymerization degree of prepolycondensate sends in whole polycondensation vessel D05 by transferpump, on the connecting tube of precondensation still D04 and whole polycondensation vessel D05, arrange properties-correcting agent adder (such as: syringe) and static mixer, to facilitate before the eventually poly-stage, add properties-correcting agent.Prepolycondensate is in whole polycondensation vessel D05, under heating agent (thermal oil) heating and high vacuum condition, constantly deviate from small molecules, further there is polycondensation, the reaction parameter arranging in whole polycondensation vessel D05 is: temperature of reaction is 240～245 ℃, reaction pressure is 50～100Pa (absolute pressure), and the residence time is 2 hours.Under the parameter in this temperature, pressure, reaction times is controlled, when touching the mark, the polymerization degree of final minification polymers sends into viscosity-increasing reactor D06 (can be understood as tackify polycondensation vessel) by transferpump, in viscosity-increasing reactor D06, final minification polymers is constantly deviate from small molecules under heat-conducting oil heating and high vacuum condition, further there is polycondensation, make product reach higher viscosity requirement.The small molecules that reaction is deviate from is extracted out by vacuum system by gas phase pipeline, condensing works (such as condensation spray thrower) is set on gas phase pipeline, condensed gas is collected, uncondensable tail gas is taken away by vacuum pump, the reaction parameter of controlling in viscosity-increasing reactor D06 is: temperature of reaction is 245 ℃, reaction pressure 30～50Pa (absolute pressure), the residence time is 1 hour.The melt pumping from viscosity-increasing reactor D06 is sent into fondant filter after static mixer, through fondant filter, filters out 40u aggregated particle and impurity, send dry, the packing of weighing afterwards through dicing machine D08 pelletizing, wind.Wherein, the esterification occurring in the first esterifying kettle D02, second esterification kettle D03 is shown in reaction formula one; Reaction formula two is shown in the polycondensation occurring in precondensation still D04, whole polycondensation vessel D05, viscosity-increasing reactor D06.
It should be noted that:
1. esterification is different with the catalyzer adopting in polycondensation, is respectively esterifying catalyst, polycondensation catalyst, and these catalyzer can be blended into and in BDO, be prepared into BDO slurry and add.In order to improve productive rate, BDO circulation device is set in this production unit, in the gas that in the first esterifying kettle D02, second esterification kettle D03, precondensation still D04, whole polycondensation vessel D05, viscosity-increasing reactor D06, vacuum is extracted out, contain the BDO steam of condensability, the gas containing condensability BDO steam that vacuum is extracted out, by spray condenser, use cold cycle BDO to spray, BDO in steam is trapped, be stored into BDO storage tank, after filtering, for spray condenser, spray or deliver to BDO withdrawing can as raw material.The tail gas that can not be condensed in spray condenser is taken away by airless injection system.
2. the first esterifying kettle D02, second esterification kettle D03, precondensation still D04, whole polycondensation vessel D05, viscosity-increasing reactor D06 are all furnished with vacuum system, with the small molecules in extraction, water, THF etc.
3. the first esterifying kettle D02, second esterification kettle D03, precondensation still D04, whole polycondensation vessel D05, viscosity-increasing reactor D06 are all furnished with well heater, and this well heater is generally gas heat conducting oil stove, and heating agent is thermal oil.
The main performance index of poly butylene succinate (PBS) resin of preparation is in Table 1, and quality index is in Table 2:
The salient features of table 1 poly butylene succinate (PBS) resin
The main quality index of table 2 poly butylene succinate (PBS)
Reaction formula one (esterification):
Reaction formula two (polycondensation):
Succinic acid and BDO, under catalyst action, react by condensation polymerization, directly obtain high molecular weight poly (butylene succinate).Single stage method is by diprotic acid (succinic acid) and the reaction of dibasic alcohol (BDO) direct condensation, without follow-up chain extension process.Adopt the product of One-step production, avoid the isocyanato introduced because of chain extension because of, improved the food safety performance of product, for the application of product in fields such as food, drug packaging, agriculture productions provides may.The single stage method of succinic acid and the reaction of BDO direct condensation, in Technology, economic target, the aspects such as product performance have significant advantage.Polyreaction is stable, organism all reclaims in production process, is the friendly process process that meets national environmental protection regulation, and has operational performance and the experience of other industrialized unit.
The foregoing is only preferred embodiment of the present utility model, be not limited to the utility model, for a person skilled in the art, the utility model can have various modifications and variations.All within spirit of the present utility model and principle, any modification of doing, be equal to replacement, improvement etc., within all should being included in protection domain of the present utility model.
Claims (8)
1. a production unit for poly butylene succinate, is characterized in that, comprising: by pipeline successively connected slurry modulation tank, the first esterifying kettle, second esterification kettle, precondensation still, whole polycondensation vessel, viscosity-increasing reactor; Wherein,
Described slurry modulation tank is connected with succinic acid squirt pump, BDO transport pipe, catalyzer duct respectively;
Described the first esterifying kettle, described second esterification kettle are respectively equipped with esterification steam outlet, two described esterification steam outlets are all connected with the isolate entrance of knockout tower by pipeline, and the heavy constituent outlet of described knockout tower is connected with the component regenerant entrance of described the first esterifying kettle, described second esterification kettle by pipeline;
On the pipeline between described second esterification kettle and described precondensation still, be provided with transferpump and oligopolymer well heater;
On the pipeline between described precondensation still and described whole polycondensation vessel, properties-correcting agent adder and static mixer are set;
Described precondensation still, described whole polycondensation vessel, described viscosity-increasing reactor are connected with vacuum system by gas phase pipeline respectively, on described gas phase pipeline, condensing works are set;
Described viscosity-increasing reactor is provided with melt outlet, and described melt outlet is connected by melt pipe with the melt inlet of fondant filter.
2. the production unit of poly butylene succinate as claimed in claim 1, is characterized in that, described properties-correcting agent adder is syringe or squirt pump.
3. the production unit of poly butylene succinate as claimed in claim 1, is characterized in that, on described melt pipe, static mixer is set.
4. the production unit of poly butylene succinate as claimed in claim 1, is characterized in that, also comprises dicing machine, and described dicing machine is connected with described fondant filter.
5. the production unit of poly butylene succinate as claimed in claim 1, is characterized in that, described condensing works is spray condenser, and low temperature BDO is housed in described spray condenser.
6. the production unit of the poly butylene succinate as described in claim 1-5 any one, is characterized in that, described the first esterifying kettle, described second esterification kettle, described precondensation still, described whole polycondensation vessel, described viscosity-increasing reactor are equipped with well heater.
7. the production unit of poly butylene succinate as claimed in claim 6, is characterized in that, described well heater is gas heat conducting oil stove.
8. the production unit of the poly butylene succinate as described in claim 1-5 any one, is characterized in that, the light constituent outlet of described knockout tower is connected by pipeline with the regenerant entrance of tetrahydrofuran (THF) recovery system.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104549096A (en) * | 2015-01-05 | 2015-04-29 | 福建省鑫东华实业有限公司 | Heat medium heating device and heating method of prepolymerization kettle |
| CN106978638A (en) * | 2017-03-30 | 2017-07-25 | 桐昆集团股份有限公司 | A kind of integrated combined unit in Direct-spinning of PET Fiber workshop |
| CN111423570A (en) * | 2020-05-20 | 2020-07-17 | 北京芯友工程技术有限公司 | Process method and device for continuously producing degradable polyester |
| CN112159302A (en) * | 2020-11-09 | 2021-01-01 | 天津渤化工程有限公司 | Integral integrated high-temperature direct chlorination system and method |
-
2014
- 2014-07-21 CN CN201420404696.XU patent/CN203938629U/en active Active
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104549096A (en) * | 2015-01-05 | 2015-04-29 | 福建省鑫东华实业有限公司 | Heat medium heating device and heating method of prepolymerization kettle |
| CN106978638A (en) * | 2017-03-30 | 2017-07-25 | 桐昆集团股份有限公司 | A kind of integrated combined unit in Direct-spinning of PET Fiber workshop |
| CN111423570A (en) * | 2020-05-20 | 2020-07-17 | 北京芯友工程技术有限公司 | Process method and device for continuously producing degradable polyester |
| CN112159302A (en) * | 2020-11-09 | 2021-01-01 | 天津渤化工程有限公司 | Integral integrated high-temperature direct chlorination system and method |
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Address after: 032300, Lvliang, Shanxi province Xiaoyi City Indus Industrial Park Jinhui long hi tech Polytron Technologies Inc Patentee after: Jin Hui long trillion hi tech Polytron Technologies Inc Address before: 032300 Xiaoyi Lvliang Shanxi Phoenix Industrial Park Jinhui Hi Tech Co., Ltd. Patentee before: JINHUI ZHAOLONG HIGH-TECH CO., LTD. |
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Effective date of registration: 20220401 Granted publication date: 20141112 |
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