A kind of technology of preparing of PCT/PET copolyesters high molecular material
Technical field
The invention belongs to high-performance polyester technical field of modification, and in particular to a kind of PCT/PET copolyesters high molecular material
Technology of preparing.
Background technique
Dyeability is one important indicator of fibrous material, and PET is the one kind being most widely used in polyester material field
Material, the present invention improve polymerization technique and using the catalyst preparation one kind having no toxic side effect by new Molecular Design
With the high novel PCT/PET copolyester material of dyeability.It is actually rare about the report of copolyester material at present, You Renjian
The high molecular materials blending such as PCT, PBT singlely is prepared into the defect that a kind of composite material fundamentally solves polyester material,
Being improved just with its good compatibility, promotion dynamics is limited, the problem of polyester material dyeability difference can not be improved,
The invention patent prepares that a kind of have can low temperature dyeing by the preparation of novel copolymerized ester a kind of, by the way that new polymerized monomer is added
And the new polyester material that dye-uptake is high, and the development of polyester new material can also be stimulated.
Summary of the invention
The purpose of this section is to summarize some aspects of the embodiment of the present invention and briefly introduce some preferable implementations
Example.It may do a little simplified or be omitted to avoid our department is made in this section and the description of the application and the title of the invention
Point, the purpose of abstract of description and denomination of invention it is fuzzy, and this simplification or omit and cannot be used for limiting the scope of the invention.
In view of the technological gap of the technology of preparing of above-mentioned and/or existing PCT/PET copolyesters high molecular material, this is proposed
Invention.
Therefore, the purpose of the present invention is to solve deficiency in the prior art, a kind of PCT/PET copolyesters macromolecule material is provided
The technology of preparing of material.
In order to solve the above technical problems, the present invention provides the following technical scheme that a kind of PCT/PET copolyesters macromolecule material
The technology of preparing of material, including, by phthalic acid, ethylene glycol, 1,4-CHDM stirs esterification, and titanium catalyst is added, stirs
Mix polymerization reaction.
A kind of preferred embodiment of technology of preparing as PCT/PET copolyesters high molecular material of the present invention, in which: institute
Titanium catalyst, including titanium dichloride load titanium ethylene glycolate are stated, silicon dioxide carried titanium ethylene glycolate or nano montmorillonite load second two
One or more of alcohol titanium.
A kind of preferred embodiment of technology of preparing as PCT/PET copolyesters high molecular material of the present invention, in which: institute
State titanium catalyst, be titanium dichloride load titanium ethylene glycolate and nano montmorillonite load titanium ethylene glycolate 1:1 in mass ratio it is compound and
At.
A kind of preferred embodiment of technology of preparing as PCT/PET copolyesters high molecular material of the present invention, in which: institute
Titanium catalyst is stated, additive amount is 100~1000ppm.
A kind of preferred embodiment of technology of preparing as PCT/PET copolyesters high molecular material of the present invention, in which: institute
Esterification is stated, temperature is 200~300 DEG C, and pressure is 20~25KPa, is esterified 2~8h.
A kind of preferred embodiment of technology of preparing as PCT/PET copolyesters high molecular material of the present invention, in which: institute
Polymerization reaction is stated, temperature is 250~360 DEG C, and pressure is 1~5KPa, and the reaction time is 2~12h.
A kind of preferred embodiment of technology of preparing as PCT/PET copolyesters high molecular material of the present invention, in which: institute
The mass ratio for stating phthalic acid and ethylene glycol is 10:1~9.
A kind of preferred embodiment of technology of preparing as PCT/PET copolyesters high molecular material of the present invention, in which: institute
The mass ratio for stating phthalic acid and 1,4 cyclohexane dimethanol is 10:1~9.
A kind of preferred embodiment of technology of preparing as PCT/PET copolyesters high molecular material of the present invention, in which: institute
Stirring esterification is stated, mixing speed is 200~400r/min.
A kind of preferred embodiment of technology of preparing as PCT/PET copolyesters high molecular material of the present invention, in which: institute
Stirring polymerization reaction is stated, mixing speed is 200~400r/min.
Possessed by of the invention the utility model has the advantages that
(1) copolyester material produced by the present invention has higher mechanical performance, dyeability and heat resistance.
(2) polyester material produced by the present invention is polymerize by novel catalyst system, so that product colour quality ten
Divide outstanding.
Detailed description of the invention
In order to illustrate the technical solution of the embodiments of the present invention more clearly, required use in being described below to embodiment
Attached drawing be briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention, for this
For the those of ordinary skill of field, without any creative labor, it can also be obtained according to these attached drawings other
Attached drawing.Wherein:
Fig. 1 is the heat resistance test of copolyester material made from embodiment 1;
Fig. 2 is the heat resistance test of copolyester material made from embodiment 2.
Specific embodiment
In order to make the foregoing objectives, features and advantages of the present invention clearer and more comprehensible, right combined with specific embodiments below
A specific embodiment of the invention is described in detail.
In the following description, numerous specific details are set forth in order to facilitate a full understanding of the present invention, but the present invention can be with
Implemented using other than the one described here other way, those skilled in the art can be without prejudice to intension of the present invention
In the case of do similar popularization, therefore the present invention is not limited by the specific embodiments disclosed below.
Secondly, " one embodiment " or " embodiment " referred to herein, which refers to, may be included at least one realization side of the invention
A particular feature, structure, or characteristic in formula." in one embodiment " that different places occur in the present specification not refers both to
The same embodiment, nor the individual or selective embodiment mutually exclusive with other embodiments.
Embodiment 1
(1) raw material prepare: selection technical grade terephthalic acid (TPA), ethylene glycol, 1,4-CHDM are sealed;
(2) enzymatic synthesis condition is arranged: using vacuum pressure reaction kettle, polymerization raw material is fed intake according to a certain percentage, herein
Ratio of the terephthalic acid (TPA) compared to ethylene glycol and 1,4-CHDM are as follows: 10:9:1, heating, in 270 DEG C, pressure
Esterification 2h under 20KPa, mixing speed 200rpm.
(3) polymerizing condition is arranged: after esterification, titanium dichloride load titanium ethylene glycolate is added, nano montmorillonite loads second
Glycol titanium compounds Titanium series catalyst, and the additive amount of mass ratio 1:1, catalyst are 1000ppm, at 280 DEG C, pressure 3KPa
Polymerization reaction 2h, mixing speed 400rpm, are made polymer sample, and color is white.
Polymer sample is prepared into fiber by spinning, by the insertion of PCT unit, sample initial decomposition temperature is at 400 DEG C
Left and right, peak value is at 412 DEG C, and heat distortion temperature is promoted by 70 DEG C of PET to 72 DEG C, and the promotion of softening point means using temperature
Can increase, mechanical property is as shown in the table:
Sample |
Strongly (CN) |
Extension at break mm |
Elongation % |
1# |
403.7 |
24.326 |
9.727 |
It is as shown in the table that color fastness value is tested after fiber weaving fabric made from the present embodiment 1:
Embodiment 2
(1) raw material prepare: selection technical grade terephthalic acid (TPA), ethylene glycol, 1,4-CHDM are sealed;
(2) enzymatic synthesis condition is arranged: using vacuum pressure reaction kettle, polymerization raw material is fed intake according to a certain percentage, herein
Ratio of the terephthalic acid (TPA) compared to ethylene glycol and 1,4-CHDM are as follows: 10:1:9, heating, in 270 DEG C, pressure
Esterification 2h under 20KPa, mixing speed 200rpm.
(3) polymerizing condition is arranged: after esterification, titanium dichloride load titanium ethylene glycolate is added, nano montmorillonite loads second
Glycol titanium compounds Titanium series catalyst, and the additive amount of mass ratio 1:1, catalyst are 1000ppm, at 280 DEG C, pressure 3KPa
Polymerization reaction 2h, mixing speed 300rpm, are made polymer sample, and color is white.
Polymer sample prepares fiber by spinning, and by the insertion of PCT unit, sample initial decomposition temperature is on 400 DEG C of left sides
The right side, peak value is at 414 DEG C, and heat distortion temperature is promoted by 70 DEG C of PET to 82 DEG C, and the promotion of softening point means using temperature
It can increase, mechanical property is as shown in the table:
Sample |
Strongly (CN) |
Extension at break mm |
Elongation % |
2# |
454.8 |
23.907 |
9.558 |
It is as shown in the table that color fastness value is tested after fiber weaving fabric made from the present embodiment 2:
Embodiment 3
(1) raw material prepare: selection technical grade terephthalic acid (TPA), ethylene glycol, 1,4-CHDM are sealed;
(2) enzymatic synthesis condition is arranged: using vacuum pressure reaction kettle, polymerization raw material is fed intake according to a certain percentage, herein
Ratio of the terephthalic acid (TPA) compared to ethylene glycol and 1,4-CHDM are as follows: 10:5:5, heating, in 280 DEG C, pressure
Esterification 4h under 20KPa, mixing speed 200rpm.
(3) polymerizing condition is arranged: after esterification, titanium dichloride load titanium ethylene glycolate is added, nano montmorillonite loads second
Glycol titanium compounds Titanium series catalyst, and the additive amount of mass ratio 1:1, catalyst are 1000ppm, at 270 DEG C, pressure 3KPa
Polymerization reaction 2h, mixing speed 200rpm, are made polymer sample, and color is white.
Mechanical property is as shown in the table:
Sample |
Strongly (CN) |
Extension at break mm |
Elongation % |
3# |
432.5 |
22.302 |
10.321 |
It is as shown in the table that color fastness value is tested after fiber weaving fabric made from the present embodiment 3:
Embodiment 4
(1) raw material prepare: selection technical grade terephthalic acid (TPA), ethylene glycol, 1,4-CHDM are sealed;
(2) enzymatic synthesis condition is arranged: using vacuum pressure reaction kettle, polymerization raw material is fed intake according to a certain percentage, herein
Ratio of the terephthalic acid (TPA) compared to ethylene glycol and 1,4-CHDM are as follows: 10:5:5, heating, in 270 DEG C, pressure
Esterification 4h under 20KPa, mixing speed 200rpm.
(3) polymerizing condition is arranged: after esterification, titanium dichloride load titanium ethylene glycolate is added, nano montmorillonite loads second
Glycol titanium compounds Titanium series catalyst, and the additive amount of mass ratio 1:1, catalyst are 1000ppm, at 280 DEG C, pressure 3KPa
Polymerization reaction 4h, mixing speed 400rpm, are made polymer sample, and color is white.
Mechanical property is as shown in the table:
Sample |
Strongly (CN) |
Extension at break mm |
Elongation % |
4# |
452.7 |
21.254 |
10.022 |
It is as shown in the table that color fastness value is tested after fiber weaving fabric made from the present embodiment 4:
Embodiment 5
(1) raw material prepare: selection technical grade terephthalic acid (TPA), ethylene glycol, 1,4-CHDM are sealed;
(2) enzymatic synthesis condition is arranged: using vacuum pressure reaction kettle, polymerization raw material is fed intake according to a certain percentage, herein
Ratio of the terephthalic acid (TPA) compared to ethylene glycol and 1,4-CHDM are as follows: 10:5:5, heating, in 280 DEG C, pressure
Esterification 4h under 20KPa, mixing speed 200rpm.
(3) polymerizing condition is arranged: after esterification, titanium dichloride load titanium ethylene glycolate is added, nano montmorillonite loads second
Glycol titanium compounds Titanium series catalyst, and the additive amount of mass ratio 1:1, catalyst are 1000ppm, at 290 DEG C, pressure 3KPa
Polymerization reaction 4h, mixing speed 200rpm, are made polymer sample, and color is white.
Mechanical property is as shown in the table:
Sample |
Strongly (CN) |
Extension at break mm |
Elongation % |
5# |
442.7 |
20.754 |
9.985 |
It is as shown in the table that color fastness value is tested after fiber weaving fabric made from the present embodiment 5:
Embodiment 6
(1) raw material prepare: selection technical grade terephthalic acid (TPA), ethylene glycol, 1,4-CHDM are sealed;
(2) enzymatic synthesis condition is arranged: using vacuum pressure reaction kettle, polymerization raw material is fed intake according to a certain percentage, herein
Ratio of the terephthalic acid (TPA) compared to ethylene glycol and 1,4-CHDM are as follows: 10:5:5, heating, in 300 DEG C, pressure
Esterification 4h under 20KPa, mixing speed 200rpm.
(3) polymerizing condition is arranged: after esterification, titanium dichloride load titanium ethylene glycolate is added, nano montmorillonite loads second
Glycol titanium compounds Titanium series catalyst, and the additive amount of mass ratio 1:1, catalyst are 1000ppm, at 360 DEG C, pressure 3KPa
Polymerization reaction 4h, mixing speed 200rpm, are made polymer sample, and color is white.
Mechanical property is as shown in the table:
Sample |
Strongly (CN) |
Extension at break mm |
Elongation % |
3# |
279.5 |
18.254 |
8.364 |
It is as shown in the table that color fastness value is tested after fiber weaving fabric made from the present embodiment 6:
It is noted that we invents the outstanding catalyst for searching out a kind of PCT/PET copolyesters preparation, i.e. titanium dioxide
Titanium loads titanium ethylene glycolate, and nano montmorillonite loads titanium ethylene glycolate and compounds by 1:1.Our invention find under study for action titanium dioxide with
Two kinds of carriers of nano montmorillonite carry titanium ethylene glycolate, both carriers can generate synergistic effect, change catalyst morphology and lead to
It crosses mass transfer and the redistribution of interface charge carrys out the state in modulation activated centre, along with preferred, the energy of mixing speed
Enough to promote heat uniformly and melt flows, this makes activated centre state more unified, has prevented because activated centre activity is different
And the local reaction that occurs it is bad caused by lead to the problem of chromophoric group, and titanium ethylene glycolate its surface nature can be mentioned significantly
The selectivity of high reactive polymeric, so that the dyeability and mechanical performance of fabric are all very outstanding, it is not in traditional preparation
The product occurred when the middle associated catalysts using titanium turns to be yellow or in yellow.
In conclusion copolyester material produced by the present invention has higher mechanical performance, dyeability and temperature tolerance
Energy.Polyester material produced by the present invention is polymerize by novel catalyst system, so that product colour quality is very outstanding.
It should be noted that the above examples are only used to illustrate the technical scheme of the present invention and are not limiting, although referring to preferable
Embodiment describes the invention in detail, those skilled in the art should understand that, it can be to technology of the invention
Scheme is modified or replaced equivalently, and without departing from the spirit and scope of the technical solution of the present invention, should all be covered in this hair
In bright scope of the claims.