CN105085886A - Preparation method of poly(butylene succinate) - Google Patents
Preparation method of poly(butylene succinate) Download PDFInfo
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- CN105085886A CN105085886A CN201510455068.3A CN201510455068A CN105085886A CN 105085886 A CN105085886 A CN 105085886A CN 201510455068 A CN201510455068 A CN 201510455068A CN 105085886 A CN105085886 A CN 105085886A
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Abstract
The invention discloses a preparation method of poly(butylene succinate). The method comprises the steps that 1, 1,4-butanediol and butanedioic acid are sequentially added into a reaction kettle, and under the condition that double catalysts exist, diphenyl ether, p-toluenesulfonic acid and titanium isopropoxide are added for reaction; 2, an obtained solution is heated under the situation of continuous stirring, and then prepolymer is obtained after vacuum polycondensation is conducted; 3, chain extender is added into the obtained prepolymer under the condition of continuous stirring; 4, after stirring is completed, obtained product is dissolved in trichloromethane, standing precipitation is conducted till the product are fully precipitated, suction filtration and drying are conducted, and the poly(butylene succinate) is obtained. By means of the preparation method of the poly(butylene succinate), the molecular weight of the finished product is increased, and therefore the mechanical properties of the PBS are effectively improved; meanwhile, byproducts produced in the preparation process are fewer, the reaction time is shortened, the production time is shortened, the production efficiency is improved, therefore, the production cost is reduced, and the economic benefit is increased; in addition, the appearance and the properties of the finished product are excellent, and the prepared product can be widely applied to the field of chemical industry.
Description
Technical field
The present invention relates to aliphatic polyester preparing technical field, be specifically related to a kind of preparation method of poly butylene succinate.
Background technology
Along with the development of science and technology, improving constantly of people's living standard.Development and life with problem of environmental pollution be on the rise, particularly white pollution problems, become a kind of global problem, biodegradable plastic gets more and more people's extensive concerning all the more.
Due to the non-biodegradable of traditional polyolefin plastics, waste plastic is caused to cause severe contamination to environment, in order to reduce this pollution, research direction has been turned to degradative plastics by people, poly butylene succinate (PBS) is obtained through polycondensation by succinic acid and butyleneglycol, is the aliphatic polyester plastics that a kind of biodegradability is good, compared with other biological degradable plastics, PBS resistance toheat is good, and heat-drawn wire is close to 100 degrees Celsius.Current preparation method is in esterification process, and esterification temperature is 140 degrees Celsius, but when reacting at this temperature, water molecules is difficult to be distilled out of, and esterification effect is not fine.And product colour outward appearance is dark, and proterties is bad, productive rate is not high simultaneously, affects the market application of PBS.
Therefore, for the problems referred to above, the present invention proposes a kind of new technical scheme.
Summary of the invention
The object of this invention is to provide a kind of simple to operate, preparation method of poly butylene succinate of enhancing productivity.
The present invention is achieved through the following technical solutions:
A preparation method for poly butylene succinate, comprises the following steps:
A, BDO, succinic acid are added successively in reactor, under the condition of dual catalyst, add phenyl ether, tosic acid and titanium isopropoxide, then under vacuum, temperature rises to 130 ~ 160 DEG C, reaction 1 ~ 1.5h;
B, then gained solution temperature when Keep agitation is risen to 220 DEG C ~ 250 DEG C, then vacuum polycondensation 1.5 ~ 2h, obtains prepolymer;
C, gained prepolymer is added chainextender under conditions in continuous stirring, temperature controls at 100 ~ 150 DEG C, and churning time is 25 ~ 45min;
D, stirred after products therefrom is dissolved in trichloromethane, then staticly settle 2 ~ 5h, after product is separated out completely, extract required product by the mode of suction filtration, be dried to constant weight, namely obtain required finished product poly butylene succinate.
Further, the mass ratio of described BDO, succinic acid, phenyl ether, tosic acid, titanium isopropoxide is: 99 ~ 110:90 ~ 100:0.05 ~ 0.1:0.15 ~ 0.2:0.08 ~ 0.12.
Further, mass percent shared by described dual catalyst is 0.5% ~ 2% of BDO.
Further, mass percent shared by described chainextender is 1% ~ 3% of prepolymer.
Further, described chainextender is MOCA, diethylaminoethanol, quadrol one wherein.
The invention has the beneficial effects as follows: this process structure is reasonable, simple to operate, improves the molecular weight of finished product, thus effectively improve the mechanical property of PBS, meanwhile, it is few that this preparation process bears product, reaction times shortens, reduce the production time, improve production efficiency, thus reduce production cost, improve economic benefit, and finished appearance and excellent performance, can be widely used in chemical field.
Embodiment
Below in conjunction with embodiment, the present invention is described further.
Embodiment 1
A kind of preparation method of poly butylene succinate, comprise the following steps: a, by 1,4-butyleneglycol, succinic acid add in reactor successively, under the condition of dual catalyst, add phenyl ether, tosic acid and titanium isopropoxide, then under vacuum, temperature rises to 130 DEG C, reaction 1h, 1, the mass ratio of 4-butyleneglycol, succinic acid, phenyl ether, tosic acid, titanium isopropoxide is: 99:90:0.05:0.15:0.08, and mass percent shared by dual catalyst is 0.5% of BDO; B, then gained solution temperature when Keep agitation is risen to 220 DEG C, then vacuum polycondensation 1.5h, obtains prepolymer; C, gained prepolymer is added MOCA under conditions in continuous stirring, temperature controls at 100 DEG C, and churning time is mass percent shared by 25min, MOCA is 1% of prepolymer; D, stirred after products therefrom is dissolved in trichloromethane, then staticly settle 2h, after product is separated out completely, extract required product by the mode of suction filtration, be dried to constant weight, namely obtain required finished product poly butylene succinate.
Embodiment 2
A kind of preparation method of poly butylene succinate, comprise the following steps: a, by 1,4-butyleneglycol, succinic acid add in reactor successively, under the condition of dual catalyst, add phenyl ether, tosic acid and titanium isopropoxide, then under vacuum, temperature rises to 140 DEG C, reaction 1.2h, 1, the mass ratio of 4-butyleneglycol, succinic acid, phenyl ether, tosic acid, titanium isopropoxide is: 104.5:95:0.08:0.18:0.1, and mass percent shared by dual catalyst is 1% of BDO; B, then gained solution temperature when Keep agitation is risen to 230 DEG C, then vacuum polycondensation 1.8h, obtains prepolymer; C, gained prepolymer is added diethylaminoethanol under conditions in continuous stirring, temperature controls at 130 DEG C, and churning time is 30min, and mass percent shared by diethylaminoethanol is 2% of prepolymer; D, stirred after products therefrom is dissolved in trichloromethane, then staticly settle 3h, after product is separated out completely, extract required product by the mode of suction filtration, be dried to constant weight, namely obtain required finished product poly butylene succinate.
Embodiment 3
A kind of preparation method of poly butylene succinate, comprise the following steps: a, by 1,4-butyleneglycol, succinic acid add in reactor successively, under the condition of dual catalyst, add phenyl ether, tosic acid and titanium isopropoxide, then under vacuum, temperature rises to 160 DEG C, reaction 1.5h, 1, the mass ratio of 4-butyleneglycol, succinic acid, phenyl ether, tosic acid, titanium isopropoxide is: 110:100:0.1:0.2:0.12, and mass percent shared by dual catalyst is 2% of BDO; B, then gained solution temperature when Keep agitation is risen to 250 DEG C, then vacuum polycondensation 2h, obtains prepolymer; C, gained prepolymer is added quadrol under conditions in continuous stirring, temperature controls at 150 DEG C, and churning time is 45min, and mass percent shared by quadrol is 3% of prepolymer; D, stirred after products therefrom is dissolved in trichloromethane, then staticly settle 5h, after product is separated out completely, extract required product by the mode of suction filtration, be dried to constant weight, namely obtain required finished product poly butylene succinate.
This process structure is reasonable, simple to operate, improves the molecular weight of finished product, thus effectively improve the mechanical property of PBS, meanwhile, it is few that this preparation process bears product, reaction times shortens, reduce the production time, improve production efficiency, thus reduce production cost, improve economic benefit, and finished appearance and excellent performance, can be widely used in chemical field.
Although above-mentioned, the specific embodiment of the present invention is described; but not limiting the scope of the invention; on the basis of technical scheme of the present invention, those skilled in the art do not need to pay various amendment or distortion that creative work can make still within protection scope of the present invention.
Claims (5)
1. a preparation method for poly butylene succinate, is characterized in that: comprise the following steps:
A, BDO, succinic acid are added successively in reactor, under the condition of dual catalyst, add phenyl ether, tosic acid and titanium isopropoxide, then under vacuum, temperature rises to 130 ~ 160 DEG C, reaction 1 ~ 1.5h;
B, then gained solution temperature when Keep agitation is risen to 220 DEG C ~ 250 DEG C, then vacuum polycondensation 1.5 ~ 2h, obtains prepolymer;
C, gained prepolymer is added chainextender under conditions in continuous stirring, temperature controls at 100 ~ 150 DEG C, and churning time is 25 ~ 45min;
D, stirred after products therefrom is dissolved in trichloromethane, then staticly settle 2 ~ 5h, after product is separated out completely, extract required product by the mode of suction filtration, be dried to constant weight, namely obtain required finished product poly butylene succinate.
2. the preparation method of a kind of poly-butyric acid butanediol ester according to claim 1, it is characterized in that: the mass ratio of described BDO, succinic acid, phenyl ether, tosic acid, titanium isopropoxide is: 99 ~ 110:90 ~ 100:0.05 ~ 0.1:0.15 ~ 0.2:0.08 ~ 0.12.
3. the preparation method of a kind of poly-butyric acid butanediol ester according to claim 1, is characterized in that: mass percent shared by described dual catalyst is 0.5% ~ 2% of BDO.
4. the preparation method of a kind of poly-butyric acid butanediol ester according to claim 1, is characterized in that: mass percent shared by described chainextender is 1% ~ 3% of prepolymer.
5. a kind of preparation method of poly-butyric acid butanediol ester according to claim 1 or 4, is characterized in that: described chainextender is MOCA, diethylaminoethanol, quadrol one wherein.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510455068.3A CN105085886A (en) | 2015-07-30 | 2015-07-30 | Preparation method of poly(butylene succinate) |
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| CN201510455068.3A CN105085886A (en) | 2015-07-30 | 2015-07-30 | Preparation method of poly(butylene succinate) |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105801818A (en) * | 2016-05-25 | 2016-07-27 | 陕西省石油化工研究设计院 | Preparation method of high-molecular-weight poly(butylene succinate) |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105801818A (en) * | 2016-05-25 | 2016-07-27 | 陕西省石油化工研究设计院 | Preparation method of high-molecular-weight poly(butylene succinate) |
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Application publication date: 20151125 |