CN106380583A - Synthetic method of reactive ageing-resistant copolyester - Google Patents
Synthetic method of reactive ageing-resistant copolyester Download PDFInfo
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- 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
- C08G63/66—Polyesters containing oxygen in the form of ether groups
- C08G63/668—Polyesters containing oxygen in the form of ether groups derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/672—Dicarboxylic acids and dihydroxy compounds
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- 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
- C08G63/60—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from the reaction of a mixture of hydroxy carboxylic acids, polycarboxylic acids and polyhydroxy compounds
- C08G63/605—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from the reaction of a mixture of hydroxy carboxylic acids, polycarboxylic acids and polyhydroxy compounds the hydroxy and carboxylic groups being bound to aromatic rings
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- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/08—Oxygen-containing compounds
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- C08K7/00—Use of ingredients characterised by shape
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- C08K7/04—Fibres or whiskers inorganic
- C08K7/10—Silicon-containing compounds
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Abstract
The invention relates to a synthetic method of reactive ageing-resistant copolyester, and belongs to the technical field of synthesis and modification of polyester. The synthetic method of reactive ageing-resistant copolyester comprises the following steps: 1, mixing organic white carbon black nano-powder, organic wollastonite raphioid nano-fibers, calcium carbonate whiskers and p-hydroxybenzoic acid with ethylene glycol, propylene glycol and butylene glycol, and carrying out closed grinding in a liquid ball mill to prepare a uniform ageing-resistant composite alcohol solution; 2, mixing organic nanometer montmorillonite, an ultraviolet ray absorber, a light stabilizer and a high temperature antioxidant with polyethylene glycol and propylene glycol, and carrying out closed grinding in a ball mill to prepare an ageing-resistant composite promoter; and 3, blending and beating the composite alcohol solution, ethylene glycol and terephthalic acid according to a certain ratio, carrying out an esterification reaction, continuously adding the ageing-resistant composite promoter in the later stage of the esterification reaction, and further carrying out condensation polymerization to prepare the reactive ageing-resistant copolyester. The copolyester has the advantages of good ageing resistance and long service life.
Description
Technical field
The present invention relates to a kind of synthetic method of response type aging resistance copolyesters, belong to polyester synthesis technical field of modification.
Background technology
Polyester Polyethylene terephthalate (PET) is by p-phthalic acid (PTA) and ethylene glycol (EG) warp
Cross the polyethylene terephthalate that polycondensation is made, polyester has higher melt temperature (Tm) and glass transition temperature
(Tg), and there is excellent combination property, it is widely used in the fields such as engineering plastics, bottle piece, thin film and polyester fiber, polyester is fine
Dimension is but also as taking fiber and industrial yarn.Polyester has the performances such as excellent uvioresistant in itself, the product being made from
It is largely used in outdoor environment, but due to the effect such as sunlight, heat, oxygen, water will be stood out of doors for a long time, under its mechanical property etc.
Fall is very fast, and service life is shorter, and ageing resistace is poor, therefore improves the ageing resistace of polyester, improves the use longevity of polyester
Life has great importance.
White carbon can consumingly uv reflectance, be added in material and can reach the purpose delaying material aging, separately
The outer high fluidity due to white carbon and small-size effect, make material surface more fine and close carefully clean, nano-particle is high-strength in addition
Degree, makes film strength greatly enhance.
Wollastonite has the physical chemistry such as good insulating properties, wearability, higher index of refraction and higher whiteness
Can, it is widely used in pottery, paint, coating, plastics, rubber, chemical industry, papermaking and as asbestos alternative etc., its conduct
Polyester filler, can improve impact strength, strengthen mobility, improve tensile strength, impact strength, improve whiteness and opacity
Deng.
Calcium carbonate crystal whisker shows significant enhancing, toughness reinforcing work for the thermoplastic such as modified plastics, rubber, fiber
With.The bending strength of product, dimensional stability, heat stability, ageing resistace can also be improved；Also can be lifted processing characteristics and
The surface smoothness of product.
UV-327 UV absorbent can consumingly absorb ultraviolet (especially wavelength is 290-400nm), thermally-stabilised
Property good, hot volatility is little, and chemical stability is good, with material component in product, untoward reaction does not occur, and compatibility is good, can be equably
Dispersion in the material, no blooming, do not ooze out, colourless, nontoxic, odorless and inexpensive, be easy to get, its these performances become excellent
Polyester modification additive.
For solving the problem of aging during polyester material uses out of doors, general employing coats aging resistance in surface of polyester
The method of agent realizing, by the method process is simple in polyester product surface-coated, low cost, but polyester product using or
Coming off with overcoat in washing process, there is antiageing effect and declines serious, the shortcoming of its poor durability in it.
Content of the invention
It is an object of the invention to overcoming the shortcomings of that prior art exists, and provide a kind of response type aging resistance copolyesters
Synthetic method, modifying agent, by copolymerization mode, is first closed mixed grinding by closed ball milling secret anti-by the method respectively
Aging resistance should be made and be combined alcoholic solution and aging resistance compound accelerant, then aging resistance is combined alcoholic solution and normal polyester monomer
Blending making beating carries out being esterified copolyreaction, in the reaction phase addition aging resistance compound accelerant, and further combined polymerization makes one
Plant response type aging resistance copolyesters, its dispersion effect is good, and the mechanical property of material is good, and ageing resistace is excellent, and good endurance.
A kind of synthetic method of response type aging resistance copolyesters that the present invention provides, it adopts following steps：
A) press mass fraction, 2-3 part is organised white carbon nano-powder, 2-3 part draw ratio is 14-16:0.5-1.5 has
Machine SiClx lime stone nano whiskers fiber, a diameter of 0.5-3um of 1-2 part characterization parameter, length are brilliant for the 5-20um Calcium Carbonate that organises
Must, 0.2-0.5 part sodium germanate, 0.4-1.2 part lauryl amine, 5-10 part P-hydroxybenzoic acid, 60-70 part ethylene glycol, 8-10 part 1,
Ammediol, 8-10 part BDO mixes, and in the airtight griding reaction 2-4 hour of 70 DEG C of agitating ball mills, obtains a kind of anti-
Aging compound alcoholic solution, 70 DEG C of heat preservation for standby use；
B) press mass fraction, 1-2 part is organised nano imvite, 0.5-0.9 part UV-327 UV absorbent, 0.2-
0.4 part of triazine -5 light stabilizer, 0.5-0.9 part high-temperature antioxidant 1098,0.2-0.4 part antimony glycol, 0.1-0.3 part protonates
Agent phosphoric acid, 0.2-0.8 part ethanolamine, 5-10 part molecular weight is 15000 Polyethylene Glycol PEG, and 5-10 part 1,3-PD PDO mixes
Close, airtight agitating ball mill griding reaction 1-2 hour under the conditions of 70 DEG C, obtain a kind of aging resistance compound accelerant, 70 DEG C true
Sky be dehydrated to water content be less than 1% when heat preservation for standby use；
C) press mass fraction, by 2-4 part step A) aging resistance that obtains is combined alcoholic solution and mixed with 6-8 part ethylene glycol, then
Carry out proportioning with 15-18 part terephthalic acid component, and making beating is blended, be heated to 70 DEG C of vacuum dehydrations, when water content is less than 1%
When be added to polyplant, carry out esterification 2 hours under 250 DEG C of temperature, pressure 0.15MPa, in normal pressure esterification-polycondensation rank
Section, is continuously added to 1-2 part by step B) the aging resistance compound accelerant prepared, and be warming up to 270 DEG C and react 50 minutes, then take out
Vacuum, carries out polycondensation reaction under 283 DEG C of temperature, absolute pressure 100Pa, and a kind of response type aging resistance copolyesters is obtained.
A kind of synthetic method of response type aging resistance copolyesters that the present invention provides, it adopts following steps：
A) press mass fraction, by 2.5 parts of white carbon nano-powders that organise, 2.5 parts of draw ratios are 15:1 organises silicon ash
Stone nano whiskers fiber, a diameter of 1.75um of 2.5 parts of characterization parameters, length organise calcium carbonate crystal whisker for 12.5um, 0.3 part of germanium
Sour sodium, 0.8 part of lauryl amine, 7 parts of P-hydroxybenzoic acid, 65 parts of ethylene glycol, 9 parts of 1,3-PDs, 9 parts of BDO mixing,
In 70 DEG C of airtight griding reactions of agitating ball mill 3 hours, obtain a kind of aging resistance and be combined alcoholic solution, 70 DEG C of heat preservation for standby use；
B) press mass fraction, by 1.5 parts of nano imvites that organise, 0.7 part of UV-327 UV absorbent, 0.3 part three
Piperazine -5 light stabilizer, 1098,0.3 part of antimony glycol of 0.7 part of high-temperature antioxidant, 0.2 part of protonating agent phosphoric acid, 0.5 part of ethanolamine,
7 parts of molecular weight are 15000 Polyethylene Glycol PEG, 7 parts of 1,3-PDs mixing, and under the conditions of 70 DEG C, airtight agitating ball mill grinds
Mill reaction 1.5 hours, obtains a kind of aging resistance compound accelerant, heat preservation for standby use when 70 DEG C of vacuum dehydration to water content are less than 1%；
C) press mass fraction, by 3 parts of steps A) aging resistance that obtains is combined alcoholic solution and mixed with 7 parts of ethylene glycol, then with 16
Part terephthalic acid component carries out proportioning, and making beating is blended, and is heated to 70 DEG C of vacuum dehydrations, adds when water content is less than 1%
To polyplant, under 250 DEG C of temperature, pressure 0.15MPa, carry out esterification 2 hours, in normal pressure esterification-polycondensation phase, connect
Continuous add 1.5 parts by step B) the aging resistance compound accelerant prepared, and be warming up to 270 DEG C and react 50 minutes, then evacuation,
Carry out polycondensation reaction under 283 DEG C of temperature, absolute pressure 100Pa, a kind of response type aging resistance copolyesters is obtained.
Beneficial effects of the present invention are mainly manifested in：
1st, the white carbon nano-powder that organises of the present invention, organise wollastonite nano whiskers fiber, UV absorbent
While being added in raising material ageing-resistant performance, improve the flow processability of polyester fondant Deng modifying agent；Calcium Carbonate is brilliant
The addition of the modifying agent such as palpus, serves the effect of activeness and quietness；
2nd, the present invention adopts the modifying agent of ball-milling technology preparation to participate in copolymerization, and its dispersive property is good, product quality
With performance long time stability, overcome conventional property-modifying additive dispersion inequality, side reaction increase and melt processability and decline
Problem.Preferable processing characteristics is possessed by the modified polyester of the inventive method, outdoor utility is strong, and ageing resistance is obvious
Improve, service life is obviously prolonged, and has good mechanical performance index.
Specific embodiment
Below embodiments of the invention are further described.Following examples are only carried out furtherly to the application
Bright, should not be construed as the restriction to the application.
A kind of synthetic method of response type aging resistance copolyesters of the present invention, using following steps：
A) press mass fraction, 2-3 part is organised white carbon nano-powder, 2-3 part draw ratio is 14-16:0.5-1.5 has
Machine SiClx lime stone nano whiskers fiber, a diameter of 0.5-3um of 1-2 part characterization parameter, length are brilliant for the 5-20um Calcium Carbonate that organises
Must, 0.2-0.5 part sodium germanate, 0.4-1.2 part lauryl amine, 5-10 part P-hydroxybenzoic acid, 60-70 part ethylene glycol, 8-10 part 1,
Ammediol, 8-10 part BDO mixes, and in the airtight griding reaction 2-4 hour of 70 DEG C of agitating ball mills, obtains a kind of anti-
Aging compound alcoholic solution, 70 DEG C of heat preservation for standby use；
B) press mass fraction, 1-2 part is organised nano imvite, 0.5-0.9 part UV-327 UV absorbent, 0.2-
0.4 part of triazine -5 light stabilizer, 0.5-0.9 part high-temperature antioxidant 1098,0.2-0.4 part antimony glycol, 0.1-0.3 part protonates
Agent phosphoric acid, 0.2-0.8 part ethanolamine, 5-10 part molecular weight is 15000 Polyethylene Glycol PEG, and 5-10 part 1,3-PD mixes,
Airtight agitating ball mill griding reaction 1-2 hour under the conditions of 70 DEG C, obtains a kind of aging resistance compound accelerant, and 70 DEG C of vacuum take off
Heat preservation for standby use when water to water content is less than 1%；
C) press mass fraction, by 2-4 part step A) aging resistance that obtains is combined alcoholic solution and mixed with 6-8 part ethylene glycol, then
Carry out proportioning with 15-18 part terephthalic acid component, and making beating is blended, be heated to 70 DEG C of vacuum dehydrations, when water content is less than 1%
When be added to polyplant, carry out esterification 2 hours under 250 DEG C of temperature, pressure 0.15MPa, in normal pressure esterification-polycondensation rank
Section, is continuously added to 1-2 part by step B) the aging resistance compound accelerant prepared, and be warming up to 270 DEG C and react 50 minutes, then take out
Vacuum, carries out polycondensation reaction under 283 DEG C of temperature, absolute pressure 100Pa, and a kind of response type aging resistance copolyesters is obtained.
Embodiment 1：A kind of synthetic method of response type aging resistance copolyesters, using following steps：
A) press mass fraction, by 2 parts of white carbon nano-powders that organise, 2 parts of draw ratios are 14:0.5 organises wollastonite
Nano whiskers fiber, a diameter of 0.5um of 1 part of characterization parameter, length organise calcium carbonate crystal whisker for 5um, 0.2 part of sodium germanate, and 0.4
Part lauryl amine, 5 parts of P-hydroxybenzoic acid, 60 parts of ethylene glycol, 8 parts of 1,3-PDs, 8 parts of BDOs mixing, stir at 70 DEG C
Mix the airtight griding reaction of ball mill 2 hours, obtain a kind of aging resistance and be combined alcoholic solution, 70 DEG C of heat preservation for standby use；
B) press mass fraction, by 1 part of nano imvite that organises, 0.5 part of UV-327 UV absorbent, 0.2 part of triazine-
5 light stabilizers, 1098,0.2 part of antimony glycol of 0.5 part of high-temperature antioxidant, 0.1 part of protonating agent phosphoric acid, 0.2 part of ethanolamine, 5 parts
Molecular weight is 15000 Polyethylene Glycol PEG, 5 parts of 1,3-PD mixing, and under the conditions of 70 DEG C, airtight agitating ball mill grinds instead
Answer 1 hour, obtain a kind of aging resistance compound accelerant, heat preservation for standby use when 70 DEG C of vacuum dehydration to water content are less than 1%；
C) press mass fraction, by 2 parts of steps A) aging resistance that obtains is combined alcoholic solution and mixed with 6 parts of ethylene glycol, then with 15
Part terephthalic acid component carries out proportioning, and making beating is blended, and is heated to 70 DEG C of vacuum dehydrations, adds when water content is less than 1%
To polyplant, under 250 DEG C of temperature, pressure 0.15MPa, carry out esterification 2 hours, in normal pressure esterification-polycondensation phase, connect
Continuous add 1 part by step B) the aging resistance compound accelerant prepared, and be warming up to 270 DEG C and react 50 minutes, then evacuation,
Carry out polycondensation reaction under 283 DEG C of temperature, absolute pressure 100Pa, discharging after the technological requirement of processing after meeting to melt viscosity, system
Obtain a kind of response type aging resistance copolyesters.
Embodiment 2：A kind of synthetic method of response type aging resistance copolyesters, using following steps：
A) press mass fraction, by 2.5 parts of white carbon nano-powders that organise, 2.5 parts of draw ratios are 15:1 organises silicon ash
Stone nano whiskers fiber, a diameter of 1.75um of 2.5 parts of characterization parameters, length organise calcium carbonate crystal whisker for 12.5um, 0.3 part of germanium
Sour sodium, 0.8 part of lauryl amine, 7 parts of P-hydroxybenzoic acid, 65 parts of ethylene glycol, 9 parts of 1,3-PDs, 9 parts of BDO mixing,
In 70 DEG C of airtight griding reactions of agitating ball mill 3 hours, obtain a kind of aging resistance and be combined alcoholic solution, 70 DEG C of heat preservation for standby use；
B) press mass fraction, by 1.5 parts of nano imvites that organise, 0.7 part of UV-327 UV absorbent, 0.3 part three
Piperazine -5 light stabilizer, 1098,0.3 part of antimony glycol of 0.7 part of high-temperature antioxidant, 0.2 part of protonating agent phosphoric acid, 0.5 part of ethanolamine,
7 parts of molecular weight are 15000 Polyethylene Glycol PEG, 7 parts of 1,3-PDs mixing, and under the conditions of 70 DEG C, airtight agitating ball mill grinds
Mill reaction 1.5 hours, obtains a kind of aging resistance compound accelerant, heat preservation for standby use when 70 DEG C of vacuum dehydration to water content are less than 1%；
C) press mass fraction, by 3 parts of steps A) aging resistance that obtains is combined alcoholic solution and mixed with 7 parts of ethylene glycol, then with 16
Part terephthalic acid component carries out proportioning, and making beating is blended, and is heated to 70 DEG C of vacuum dehydrations, adds when water content is less than 1%
To polyplant, under 250 DEG C of temperature, pressure 0.15MPa, carry out esterification 2 hours, in normal pressure esterification-polycondensation phase, connect
Continuous add 1.5 parts by step B) the aging resistance compound accelerant prepared, and be warming up to 270 DEG C and react 50 minutes, then evacuation,
Carry out polycondensation reaction under 283 DEG C of temperature, absolute pressure 100Pa, discharging after the technological requirement of processing after meeting to melt viscosity,
A kind of response type aging resistance copolyesters is obtained.
Embodiment 3：A kind of synthetic method of response type aging resistance copolyesters, using following steps：
A) press mass fraction, by 3 parts of white carbon nano-powders that organise, 3 parts of draw ratios are 16:1.5 organise wollastonite
Nano whiskers fiber, a diameter of 3um of 2 parts of characterization parameters, length organise calcium carbonate crystal whisker for 20um, 0.5 part of sodium germanate, and 1.2
Part lauryl amine, 10 parts of P-hydroxybenzoic acid, 70 parts of ethylene glycol, 10 parts of 1,3-PDs, 10 parts of BDOs mixing, at 70 DEG C
The airtight griding reaction of agitating ball mill 4 hours, obtains a kind of aging resistance and is combined alcoholic solution, 70 DEG C of heat preservation for standby use；
B) press mass fraction, by 2 parts of nano imvites that organise, 0.9 part of UV-327 UV absorbent, 0.4 part of triazine-
5 light stabilizers, 1098,0.4 part of antimony glycol of 0.9 part of high-temperature antioxidant, 0.3 part of protonating agent phosphoric acid, 0.8 part of ethanolamine, 10
Part molecular weight is 15000 Polyethylene Glycol PEG, 10 parts of 1,3-PDs mixing, and under the conditions of 70 DEG C, airtight agitating ball mill grinds
Mill reaction 2 hours, obtains a kind of aging resistance compound accelerant, heat preservation for standby use when 70 DEG C of vacuum dehydration to water content are less than 1%；
C) press mass fraction, by 4 parts of steps A) aging resistance that obtains is combined alcoholic solution and mixed with 8 parts of ethylene glycol, then with 18
Part terephthalic acid component carries out proportioning, and making beating is blended, and is heated to 70 DEG C of vacuum dehydrations, adds when water content is less than 1%
To polyplant, under 250 DEG C of temperature, pressure 0.15MPa, carry out esterification 2 hours, in normal pressure esterification-polycondensation phase, connect
Continuous add 2 parts by step B) the aging resistance compound accelerant prepared, and be warming up to 270 DEG C and react 50 minutes, then evacuation,
Carry out polycondensation reaction under 283 DEG C of temperature, absolute pressure 100Pa, discharging after the technological requirement of processing after meeting to melt viscosity, system
Obtain a kind of response type aging resistance copolyesters.
Embodiment of the present invention is not limited to embodiment described above, by aforementioned disclosed numerical range, just
Arbitrarily replaced in specific embodiment, such that it is able to obtain numerous embodiment, this is not enumerated.
Claims (2)
1. a kind of synthetic method of response type aging resistance copolyesters is it is characterised in that this synthetic method adopts following steps：
A) press mass fraction, 2-3 part is organised white carbon nano-powder, 2-3 part draw ratio is 14-16:0.5-1.5 organises
Wollastonite nano whiskers fiber, a diameter of 0.5-3um of 1-2 part characterization parameter, length organise calcium carbonate crystal whisker for 5-20um,
0.2-0.5 part sodium germanate, 0.4-1.2 part lauryl amine, 5-10 part P-hydroxybenzoic acid, 60-70 part ethylene glycol, 8-10 part 1,3- third
Glycol, 8-10 part BDO mixes, and in the airtight griding reaction 2-4 hour of 70 DEG C of agitating ball mills, obtains a kind of aging resistance
Compound alcoholic solution, 70 DEG C of heat preservation for standby use；
B) press mass fraction, 1-2 part is organised nano imvite, 0.5-0.9 part UV-327 UV absorbent, 0.2-0.4
Part triazine -5 light stabilizer, 0.5-0.9 part high-temperature antioxidant 1098,0.2-0.4 part antimony glycol, 0.1-0.3 part protonating agent
Phosphoric acid, 0.2-0.8 part ethanolamine, 5-10 part molecular weight is 15000 Polyethylene Glycol, and 5-10 part 1,3-PD mixes, 70
Under the conditions of DEG C, airtight agitating ball mill griding reaction 1-2 hour, obtains a kind of aging resistance compound accelerant, 70 DEG C of vacuum dehydrations are extremely
Heat preservation for standby use when water content is less than 1%；
C) press mass fraction, by 2-4 part step A) aging resistance that obtains is combined alcoholic solution and mixed with 6-8 part ethylene glycol, then with 15-
18 parts of terephthalic acid component carry out proportioning, and making beating is blended, and are heated to 70 DEG C of vacuum dehydrations, add when water content is less than 1%
Enter to polyplant, under 250 DEG C of temperature, pressure 0.15MPa, carry out esterification 2 hours, in normal pressure esterification-polycondensation phase,
It is continuously added to 1-2 part by step B) the aging resistance compound accelerant prepared, and be warming up to 270 DEG C and react 50 minutes, then take out true
Sky, carries out polycondensation reaction under 283 DEG C of temperature, absolute pressure 100Pa, and a kind of response type aging resistance copolyesters is obtained.
2. a kind of synthetic method of response type aging resistance copolyesters is it is characterised in that this manufacture method adopts following steps：
A) press mass fraction, by 2.5 parts of white carbon nano-powders that organise, 2.5 parts of draw ratios are 15:1 wollastonite that organises is received
Rice raphioid fiber, a diameter of 1.75um of 2.5 parts of characterization parameters, length organise calcium carbonate crystal whisker for 12.5um, 0.3 part of germanic acid
Sodium, 0.8 part of lauryl amine, 7 parts of P-hydroxybenzoic acid, 65 parts of ethylene glycol, 9 parts of 1,3-PDs, 9 parts of BDO mixing,
70 DEG C of airtight griding reactions of agitating ball mill 3 hours, obtain a kind of aging resistance and are combined alcoholic solution, 70 DEG C of heat preservation for standby use；
B) press mass fraction, by 1.5 parts of nano imvites that organise, 0.7 part of UV-327 UV absorbent, 0.3 part of triazine -5
Light stabilizer, 1098,0.3 part of antimony glycol of 0.7 part of high-temperature antioxidant, 0.2 part of protonating agent phosphoric acid, 0.5 part of ethanolamine, 7 parts
Molecular weight is 15000 Polyethylene Glycol, 7 parts of 1,3-PD mixing, airtight agitating ball mill griding reaction under the conditions of 70 DEG C
1.5 hours, obtain a kind of aging resistance compound accelerant, heat preservation for standby use when 70 DEG C of vacuum dehydration to water content are less than 1%；
C) press mass fraction, by 3 parts of steps A) aging resistance that obtains is combined alcoholic solution and mixed with 7 parts of ethylene glycol, more right with 16 parts
Terephthalic acid component carries out proportioning, and making beating is blended, and is heated to 70 DEG C of vacuum dehydrations, is added to poly- when water content is less than 1%
Attach together and put, under 250 DEG C of temperature, pressure 0.15MPa, carry out esterification 2 hours, in normal pressure esterification-polycondensation phase, continuously add
Enter 1.5 parts by step B) the aging resistance compound accelerant prepared, and be warming up to 270 DEG C and react 50 minutes, then evacuation, in temperature
Carry out polycondensation reaction under 283 DEG C of degree, absolute pressure 100Pa, a kind of response type aging resistance copolyesters is obtained.
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| CN108383986A (en) * | 2018-01-23 | 2018-08-10 | 浙江省现代纺织工业研究院 | A kind of preparation method of differential PTA |
| CN108456297A (en) * | 2018-01-23 | 2018-08-28 | 浙江省现代纺织工业研究院 | A kind of preparation method of differential EG |
| CN108484887A (en) * | 2018-01-23 | 2018-09-04 | 浙江省现代纺织工业研究院 | A kind of preparation method of compound PTA |
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Application publication date: 20170208 |