CN106519202A - Micro-crystalline cellulose modified polyester preparation method - Google Patents
Micro-crystalline cellulose modified polyester preparation method Download PDFInfo
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- CN106519202A CN106519202A CN201610957299.9A CN201610957299A CN106519202A CN 106519202 A CN106519202 A CN 106519202A CN 201610957299 A CN201610957299 A CN 201610957299A CN 106519202 A CN106519202 A CN 106519202A
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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
- C08G63/66—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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B15/00—Preparation of other cellulose derivatives or modified cellulose, e.g. complexes
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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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Abstract
The invention belongs to the technical field of polyester. In order to solve the hydrophile problem of polyester, the present invention provides a micro-crystalline cellulose modified polyester preparation method. The method comprises in sequential order the steps of preparing the micro-crystalline cellulose and conducting the surface decoration, beating the micro-crystalline cellulose into pulp, and conducting the in-situ addition of the micro-crystalline cellulose. The prepared polyester had a good hydrophile property. Polyhydroxy active site can enable the fiber to be dyed under mild conditions and have an excellent dying property. The polymer can be widely used for preparing fiber with moisture absorbing, sweat dispelling and anti-static properties, and can be used as a close-fitting fabric and a high color fastness fiber product.
Description
Technical field
The present invention relates to polyester technical field, is specifically related to a kind of preparation method of Microcrystalline Cellulose modified poly ester, will
The preparation method being incorporated into after cellulose crystallite surface modification in form of slurry in polyester.
Background technology
Polyester fiber is the kind being most widely used in current synthetic fibers, and polyester molecule structural arrangement is regular, crystallization
Degree is high, this gives the good mechanical property of polyester fiber, wrinkle resistance etc..Polyester construction is while its excellent properties is given
There is shortcoming：Molecule chain alignment closely, lacks polar functional group, result in that its hygroscopicity is very poor, and moisture is difficult in the polyester
Diffusion.Under standard environment, polyester fiber regain is only 0.4%, and has substantial amounts of polar functional in cotton fiber molecular structure
Group's hydroxyl, fiber regain reach 7.5%～8.0%.Polar functional is introduced in the polyester for this method by chemical modification
Roll into a ball hydroxyl to improve its moisture pick-up properties.But multistep esterification technique is with dihydroxylic alcohols excess in traditional polyester preparation process, in
Between product all with hydroxy-end capped, the carboxyl that further can be reacted is few, is to improve the modification by copolymerization that polyester moisture pick-up propertiess add
Monomer polyhydroxy-alcohol is difficult to participate in esterification, only in the form of small molecule in polyester system, does not reach introducing many
The effect of hydroxyl modification.Method prepared by this polyester constrains the further development of polyester technology in many occasions.Such as：
Hydrophilicity, lacks polar functional group in polyester fiber strand, and under standard environment, (20 DEG C, relative humidity is
65%), regain is only 0.4%, and hygroscopicity is poor, uses as field dress is taken, is also easy to produce feeling of oppression and heat.And natural fiber cotton is fine
Contain substantial amounts of hydroxy functional group in dimension strand, regain reaches 7.5～8% under identical humiture, with good
Hygroscopicity.
Antistatic property, lacks polar functional group in polyester fiber strand, is also easy to produce the aggregation of electrostatic, causes to ash
The adsorption of dirt, causes stain resistance to decline.
Dyeability, conventional polyester fiber strand arranged regular, degree of crystallinity are high.Dye molecule hardly enters crystalline region, fine
The dyeing of dimension needs to carry out under high-temperature and high-pressure conditions, and lacks reactive functional groups in strand, the dyeing of polyester fiber
Deep dye effect is relatively inaccessible to, color fastness also can constantly decline with the time.In cotton fiber strand, reactive functionality hydroxyl can be with
Reactive dye react, and dye molecule forms firm covalent bond with hydroxyl, with high color fastness Color.
Due to lacking necessary polar functional group such as hydroxyl etc. in polyester molecule, polyester molecule chain structure arranged regular is inhaled
Moist difference, is also easy to produce sultry discomfort, is also easy to produce electrostatic phenomenon, accumulate dust；Dyeing needs to enter at high temperature under high pressure simultaneously
OK, consume substantial amounts of energy consumption.For these performances of lifting polyester fiber, copolymerization, blending, coating, surface treatment etc. has been primarily formed
Method, wherein introduces modified component in the polyester and can give polyester permanent moisture pick-up propertiess, while can lift which comprehensively taking
Use performance.It is usually used in polyester modified component and includes polyhydric alcohol, the monomer containing ionic bond, such as sulfonate etc..Wherein sulphur
The modified component of Barbiturates affects especially big to the polyester fondant mobile performance for preparing, and the fibre forming property of modified poly ester is caused
King-sized adverse effect.In terms of polyhydric alcohol is as modification by copolymerization monomer, patent US2002019508 and WO2005019301
Using Polyethylene Glycol as modification by copolymerization component, obtain that there is good hygroscopic modified poly ester and fiber.Patent W00012793 is selected
With Polyethylene Glycol, tetramethylolmethane as copolymerization component, the modified polyester fiber hydrophilicity for preparing is suitable with cotton fiber.It is many
Hydroxyl alcohol is that polyester hydrophilic co is modified the most frequently used component, for the hot wet migration for lifting polyester fiber has important meaning
Justice.
Cellulose has the advantages such as degradable, low cost, environmental friendliness, crystallite as a kind of reproducible natural polyols
Its amorphous region can be reacted away under conditions of acid by cellulose, form cellulose crystallite.Can be with by controlling reaction condition
Obtain the cellulose crystallite of specific dimensions size.The diameter that cellulose crystallite is obtained by acid hydrolysis is from several nanometers to several tens of nanometers
, the cellulose crystals of Nano grade are become into cellulose crystallite typically.Cellulose crystallite surface is rich in hydroxyl, with excellent
Water adsorption ability.Use as polyester modification, how to realize Cellulose nanocrystal uniform and stable dispersion and reservation in the polyester
It is the technical problem most merited attention in study on the modification which has the hydroxyl of absorbability.At present the research report of this respect compared with
Few, CN 201410546019.6 is reported and for Microcrystalline Cellulose to be participated in the first esterification with ethylene glycol beating, is terminated in esterification
Add polyhydroxy-alcohol afterwards again, in below 500nm, addition is 0.5-2wt% in the melt to nanocrystalline length.CN
201410545915.0 by Microcrystalline Cellulose and phosphorus flame retardant be beaten the class stage be added in carboxylate continue esterification,
Polycondensation obtains product.Size 0.5-2 μm of Microcrystalline Cellulose, addition are 3-7%.But for how cellulose crystallite avoids
Hydrolysis under high temperature and how protecting in high temperature polymerization to the hydroxyl on cellulose crystallite surface is not illustrated.
The content of the invention
For solving the hydrophilic sex chromosome mosaicism of polyester, the present invention provides a kind of preparation method of Microcrystalline Cellulose modified poly ester, improves
Polyester hydrophilicity, Microcrystalline Cellulose modified poly ester can be widely applied to prepare moisture absorbing and sweat releasing, antistatic fibre, used as next to the skin
Fabric, high color fastness fiber product.
The present invention is achieved by the following technical solutions：A kind of preparation method of Microcrystalline Cellulose modified poly ester, prepares
Sterically hindered protected effect is formed to its surface modification with phthalic acid during cellulose crystallite, then is added in form of slurry
The method being added in polyester synthesis.Hydroxyl adsorption activity due to cellulose crystallite dispersibility in the base and surface is for changing
Property polyester performance there is material impact, while cellulose is brilliant easily to occur hydrolysis under the high temperature conditions, therefore how to realize fibre
The hydrolysis that the plain crystallite of dimension good dispersion in the base, the hydroxyl on surface are not reacted away and reduced under high temperature are fibers
The key of plain crystallite application.Concretely comprise the following steps：
(1) preparation of cellulose crystallite and its surface modification
During Microcrystalline Cellulose is added to mineral acid and phthalic acid mixed acid, under oil bath constant temperature, persistently stirring is decomposed
Afterwards, deionized water cleaning obtains cellulose crystallite dispersion liquid, by dispersion liquid lyophilization, that is, obtains surface phthalic acid and repaiies
The cellulose crystallite of decorations；Described cellulose crystallite is bar-shaped or ellipticity, and grain size size is in 5-500nm.
The usage amount of mixed acid is the amount for making Microcrystalline Cellulose decompose completely, mineral acid and adjacent benzene two in described mixed acid
The mol ratio of formic acid is 1：0.1～1, preferably, mineral acid is selected from one or more in sulphuric acid, nitric acid, hydrochloric acid, its concentration
For 1-10mol/L.Mineral acid in mixed acid had both served cellulose crystallite raw material is carried out decomposing and had generated cellulose crystallite
Effect, while play a part of catalysis to the hydroxyl on cellulose crystallite surface and the esterification of phthalic acid.O-phthalic
Acid with aromatic rings, with larger sterically hindered and thermal stability, after the hydroxyl reaction on cellulose crystallite surface with
The form of chemical bond coats its surface, plays the effect of sterically hindered protection, prevents the hydroxyl reaction on cellulose crystallite surface complete
Entirely.The ability of adsorption moisture is had by the hydroxyl on protection cellulose crystallite surface, matrix hydrophilic can be strengthened.
Preferably, the control of oil bath constant temperature is at 100-120 DEG C, response time 5-10h.
(2) cellulose crystallite/dihydroxylic alcohols beating
The cellulose crystallite of surface modification is beaten in dihydroxylic alcohols, while adding phthalic anhydride, cellulose crystallite is obtained
Serosity；Cellulose crystallite and dihydroxylic alcohols mixing beating be in order to ensure that cellulose crystallite is dispersed, can in being incorporated into carboxylate
To realize stirring；
The dihydroxylic alcohols are selected from one or more in ethylene glycol, Propylene Glycol, butanediol, pentanediol, hexanediol；Surface modification
Cellulose crystallite shared mass percent in dihydroxylic alcohols is 20%-60%.
0.5%-5% of the phthalic anhydride usage amount for the cellulose crystallite quality of surface modification.The adjacent benzene two of addition
Formic anhydride is in order to the reaction of moisture that will may have in carboxylate is complete, it is to avoid cellulose crystallite is hydrolyzed at high temperature.Adjacent benzene two
Formic anhydride and water react the phthalic acid that generates and polyester and have a similar compatibility, reinforcing fiber element crystallite in the base point
Scattered property.The structural representation combined with moisture by phthalic acid modified cellulose microstructure is as follows：
(3) cellulose crystallite serosity addition in situ
Cellulose crystallite serosity that step (2) is obtained, heat stabilizer, antioxidant are added to after polyester completes the second esterification
In reactor, continue stirring esterification, polycondensation reaction, finally prepare Microcrystalline Cellulose modified poly ester.
It is to make cellulose micro- to continue stirring esterification after cellulose crystallite serosity is added in polyester esterification thing
Crystalline substance in carboxylate is sufficiently stirred for being uniformly dispersed.Can be tied with the moisture in carboxylate also for guarantee phthalic anhydride
Close, it is to avoid the hydrolysis of cellulose crystallite.
5-50% of the usage amount of cellulose crystallite serosity for p-phthalic acid quality, the addition of heat stabilizer is to benzene
The 0.001～0.02% of dioctyl phthalate quality；The addition of the antioxidant for p-phthalic acid quality 0.001～
0.03%.
The heat stabilizer be selected from phosphate compounds, preferably, selected from trimethyl phosphate, alkyl phosphoric acid diester,
One or more in three (nonyl phenyl) phosphite ester.
Preferably, antioxidant is a kind of or several in antioxidant 1010, antioxidant 168, antioxidant 616
Kind.
As preferred.It is 240～260 DEG C to continue esterification reaction temperature, and esterification continues 0.5-1.5h；Continue polycondensation anti-
The temperature answered is maintained at 260～280 DEG C, and polycondensation reaction continues 2～4h.
The present invention is in cellulose crystallite preparation process, anti-with the hydroxyl on cellulose crystallite surface using phthalic acid
Should, chemical bond is formed, phthalic acid is formed on cellulose crystallite surface and is coated.Phthalic acid has preferable space bit
Resistance, protects the hydroxyl of cellulose crystallite surface residual.Old slurry is beaten with cellulose crystallite, phthalic anhydride and dihydroxylic alcohols again
Liquid, adds when polyester completes the second Esterification Stage.Phthalic anhydride in serosity can may be remaining in carboxylate
Moisture reacts rapidly, generates phthalic acid, it is to avoid the possibility that cellulose crystallite is hydrolyzed at high temperature.Phthalic acid and polyester
With the good compatibility, the brilliant compatibility in the base of cellulose is improve.Dispersed cellulose crystallite in the polyester
Reinforced polyester mechanical property can be played, it is often more important that the rich adsorption group in cellulose crystallite surface can be tied with hydrone
Close, improve polyester hydrophilicity.
Sterically hindered protection is formed to its surface modification with phthalic acid particularly during cellulose crystallite is prepared
Effect, then the method being added in polyester synthesis in form of slurry.Due to cellulose crystallite dispersibility in the base and table
The hydroxyl adsorption activity in face has material impact for the performance of modified poly ester, while cellulose crystalline substance is easily sent out under the high temperature conditions
Unboiled water solution, therefore how to realize that cellulose crystallite good dispersion in the base, the hydroxyl on surface are not reacted away and reduced
Hydrolysis under high temperature are the keys of cellulose crystallite application.
Compared with prior art, the invention has the beneficial effects as follows：
(1) it is of the invention in cellulose crystallite preparation process, using phthalic acid and the hydroxyl reaction on cellulose crystallite surface,
Chemical bond is formed, phthalic acid is formed on cellulose crystallite surface and coated.Phthalic acid have it is preferably sterically hindered,
The hydroxyl of protection cellulose crystallite surface residual；
(2) present invention is beaten old serosity with cellulose crystallite, phthalic anhydride and ethylene glycol, completes the second esterification rank in polyester
Add during section.Possible remaining moisture in carboxylate can be reacted rapidly by the phthalic anhydride in serosity, generate adjacent benzene two
Formic acid, it is to avoid the possibility that cellulose crystallite is hydrolyzed at high temperature；
(3) phthalic acid has the good compatibility with polyester, improves the cellulose crystallite compatibility in the base.Uniformly
Dispersion cellulose crystallite in the polyester can play reinforced polyester mechanical property, it is often more important that cellulose crystallite surface is rich
Adsorption group can improve polyester hydrophilicity with water molecules.
Specific embodiment
With reference to specific embodiment, the present invention is expanded on further.Raw materials used commercially available or employing in embodiment
It is prepared by conventional method.
It should be understood that these embodiments are only illustrative of the invention and is not intended to limit the scope of the invention.In addition, it is to be understood that
After the content for having read instruction of the present invention, those skilled in the art can be made various changes or modifications to the present invention, these
The equivalent form of value equally falls within the application appended claims limited range.
Embodiment 1
(1) preparation of cellulose crystallite and its surface modification：
Microcrystalline Cellulose is added in the sulphuric acid that concentration is 10mol/L with phthalic acid mixed acid, Microcrystalline Cellulose is made
Fully decompose, sulphuric acid is 1: 0.1 with the mol ratio of phthalic acid；Under the conditions of 100 DEG C of oil bath constant temperature, persistently stirring decomposes anti-
10h, deionized water cleaning is answered to obtain cellulose crystallite dispersion liquid, by dispersion liquid lyophilization, that is, obtain grain size size
For the cellulose crystallite of the surface phthalic acid modification of 100nm.
(2) cellulose crystallite/dihydroxylic alcohols beating：
Mass fraction ratio by the cellulose crystallite of surface modification in ethylene glycol prepared by step (1) is 20% and to be beaten,
Add phthalic anhydride simultaneously, the phthalic anhydride of addition is the 5% of the cellulose crystallite quality of surface modification, forms equal
Even cellulose crystallite serosity.
(3) cellulose crystallite serosity addition in situ
By the cellulose crystallite serosity and heat stabilizer trimethyl phosphate, antioxidant 1010 after polyester completes the second esterification
It is added in reactor, the p-phthalic acid that is added to of cellulose crystallite serosity feeds intake the 10% of quality；Heat stabilizer tricresyl phosphate
The addition of methyl ester for p-phthalic acid quality 0.001%；The addition of the antioxidant 1010 is p-phthalic acid matter
The 0.001% of amount.Continue stirring esterification, polycondensation reaction, esterification reaction temperature is 250 DEG C, and esterification continues 0.5h；Contracting
The temperature of poly- reaction is maintained at 270 DEG C, and the poly- reaction continues 2.5h；Microcrystalline Cellulose modified poly ester 1 is prepared finally.
The intrinsic viscosity of the modified hydrophilic polyesters section 1 of Microcrystalline Cellulose is 0.625dL/g, and fusing point is 251.2 DEG C, section
Surface water contact angle is 56 °.
Embodiment 2
(1) preparation of cellulose crystallite and its surface modification：
Microcrystalline Cellulose is added in the hydrochloric acid and phthalic acid mixed acid that concentration is 5mol/L, makes Microcrystalline Cellulose abundant
Decompose, in mixed acid, hydrochloric acid is 1: 0.5 with the mol ratio of phthalic acid；Under oil bath constant temperature：Oil bath constant temperature control
System stirs decomposition reaction 8h at 110 DEG C, persistently, and deionized water cleaning obtains cellulose crystallite dispersion liquid, dispersion liquid is freezed
It is dried, that is, obtains the cellulose crystallite of the surface phthalic acid modification that grain size size is 150nm.
(2) cellulose crystallite/dihydroxylic alcohols beating：
The cellulose crystallite of surface modification is beaten in Propylene Glycol, cellulose crystallite matter shared by Propylene Glycol of surface modification
The 40% of amount；Add phthalic anhydride simultaneously, form uniform cellulose crystallite serosity, phthalic anhydride addition surface
The cellulose crystallite of modification for cellulose crystallite quality 0.5%.
(3) cellulose crystallite serosity addition in situ
The cellulose crystallite serosity and heat stabilizer three (nonyl phenyl) phosphite ester, antioxidant 168 are completed in polyester
It is added to after class in reactor, the addition of cellulose crystallite serosity feeds intake the 5% of quality for p-phthalic acid, thermally-stabilised
The addition of agent for p-phthalic acid quality 0.02%, the addition of antioxidant is the 0.03% of p-phthalic acid quality.
Continue stirring esterification, polycondensation reaction, esterification reaction temperature is 240 DEG C, and esterification continues 1.0h；The temperature of polycondensation reaction
It is maintained at 260 DEG C；Polycondensation reaction continues 4.0h, finally prepares Microcrystalline Cellulose modified poly ester 2.
The intrinsic viscosity of the modified hydrophilic polyesters section 2 of Microcrystalline Cellulose is 0.635dL/g, and fusing point is 249.6 DEG C, section
Surface water contact angle is 52 °.
Embodiment 3
(1) preparation of cellulose crystallite and its surface modification：
Microcrystalline Cellulose is added in the nitric acid and phthalic acid mixed acid that concentration is 1mol/L, makes Microcrystalline Cellulose abundant
Decompose, the mol ratio 1: 1 of nitric acid and phthalic acid in mixed acid, under the conditions of 120 DEG C of oil bath constant temperature, persistently stirring decomposes anti-
5h between seasonable, deionized water cleaning obtain cellulose crystallite, by dispersion liquid lyophilization, that is, obtain the cellulose crystallite
Cellulose crystallite of the grain size size for the surface phthalic acid modification of 200nm.
(2) cellulose crystallite/dihydroxylic alcohols beating：
The cellulose crystallite of surface modification is beaten in butanediol, cellulose crystallite shared mass fraction ratio in butanediol
60%；Add phthalic anhydride simultaneously, the phthalic anhydride of addition is 3% shape of the cellulose crystallite quality of surface modification
Uniformly cellulose crystallite serosity.
(3) cellulose crystallite serosity addition in situ
By the cellulose crystallite serosity and heat stabilizer trimethyl phosphate, antioxidant 616 after polyester completes the second esterification
Be added in reactor, the addition of cellulose crystallite serosity feeds intake the 50% of quality for p-phthalic acid, heat stabilizer plus
Enter amount for the 0.005% of p-phthalic acid quality；The addition of the antioxidant for p-phthalic acid quality 0.005%.
Continue stirring esterification, polycondensation reaction, esterification reaction temperature is 260 DEG C, and esterification continues 1.5h；The temperature of polycondensation reaction
It is maintained at 280 DEG C；Polycondensation reaction continues 3.0h；Microcrystalline Cellulose modified poly ester 3 is prepared finally.
The intrinsic viscosity of the modified hydrophilic polyesters section 3 of Microcrystalline Cellulose is 0.630dL/g, and fusing point is 248.9 DEG C, section
Surface water contact angle is 50 °.
Claims (9)
1. a kind of preparation method of Microcrystalline Cellulose modified poly ester, it is characterised in that concretely comprise the following steps：
（1）The preparation of cellulose crystallite and its surface modification
During Microcrystalline Cellulose is added to mineral acid and phthalic acid mixed acid, under oil bath constant temperature, persistently stirring is decomposed
Afterwards, deionized water cleaning obtains cellulose crystallite dispersion liquid, by dispersion liquid lyophilization, that is, obtains surface phthalic acid and repaiies
The cellulose crystallite of decorations；
（2）Cellulose crystallite/dihydroxylic alcohols beating
The cellulose crystallite of surface modification is beaten in dihydroxylic alcohols, while adding phthalic anhydride, cellulose crystallite is obtained
Serosity；
（3）The addition in situ of cellulose crystallite serosity
By step（2）The cellulose crystallite serosity that obtains, heat stabilizer, antioxidant are added to after polyester completes the second esterification
In reactor, continue stirring esterification, polycondensation reaction, finally prepare Microcrystalline Cellulose modified poly ester.
2. the preparation method of a kind of Microcrystalline Cellulose modified poly ester according to claim 1, it is characterised in that in mixed acid
Mineral acid is 1 with the mol ratio of phthalic acid：0.1 ~ 1, wherein mineral acid is selected from the one kind or several in sulphuric acid, nitric acid, hydrochloric acid
Kind, its concentration is 1-10mol/L.
3. a kind of preparation method of Microcrystalline Cellulose modified poly ester according to claim 1, it is characterised in that step（1）
The control of oil bath constant temperature at 100-120 DEG C, response time 5-10h.
4. a kind of preparation method of Microcrystalline Cellulose modified poly ester according to claim 1, it is characterised in that the binary
Alcohol is selected from one or more in ethylene glycol, Propylene Glycol, butanediol, pentanediol, hexanediol；The cellulose crystallite of surface modification exists
In dihydroxylic alcohols, shared mass percent is 20%-60%.
5. a kind of preparation method of Microcrystalline Cellulose modified poly ester according to claim 1, it is characterised in that O-phthalic
0.5%-5% of the anhydride usage amount for the cellulose crystallite quality of surface modification.
6. a kind of preparation method of Microcrystalline Cellulose modified poly ester according to claim 1, it is characterised in that step（3）
5-50% of the usage amount of middle cellulose crystallite serosity for p-phthalic acid quality, the addition of heat stabilizer is p-phthalic acid
The 0.001～0.02% of quality；The addition of the antioxidant for p-phthalic acid quality 0.001～0.03%.
7. the preparation method of a kind of Microcrystalline Cellulose modified poly ester according to claim 6, it is characterised in that the heat is steady
Determine agent selected from trimethyl phosphate, alkyl phosphoric acid diester, three（Nonyl phenyl）One or more in phosphite ester.
8. a kind of preparation method of Microcrystalline Cellulose modified poly ester according to claim 6, it is characterised in that the antioxygen
Agent is selected from one or more in antioxidant 1010, antioxidant 168, antioxidant 616.
9. a kind of preparation method of Microcrystalline Cellulose modified poly ester according to claim 1, it is characterised in that step（3）
Middle continuation esterification reaction temperature is 240 ~ 260 DEG C, and esterification continues 0.5-1.5h；The temperature for continuing polycondensation reaction is maintained at
260～280 DEG C, polycondensation reaction continues 2～4h.
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| CN112176452A (en) * | 2020-11-11 | 2021-01-05 | 苏州鑫极纺织有限公司 | Skin-core structure water-absorbing fiber and preparation method thereof |
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| CN102690410A (en) * | 2012-05-11 | 2012-09-26 | 浙江恒逸高新材料有限公司 | Method for producing modified polyester and fiber thereof |
| CN104371093A (en) * | 2014-10-15 | 2015-02-25 | 浙江恒逸高新材料有限公司 | Preparation method of hydrophilic flame-retardant polyester slice added with renewable microcrystalline cellulose |
| CN104404647A (en) * | 2014-10-15 | 2015-03-11 | 浙江恒逸高新材料有限公司 | Hydrophilic polyester fiber modified by cellulose nanocrystal and preparation method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102690410A (en) * | 2012-05-11 | 2012-09-26 | 浙江恒逸高新材料有限公司 | Method for producing modified polyester and fiber thereof |
| CN104371093A (en) * | 2014-10-15 | 2015-02-25 | 浙江恒逸高新材料有限公司 | Preparation method of hydrophilic flame-retardant polyester slice added with renewable microcrystalline cellulose |
| CN104404647A (en) * | 2014-10-15 | 2015-03-11 | 浙江恒逸高新材料有限公司 | Hydrophilic polyester fiber modified by cellulose nanocrystal and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112176452A (en) * | 2020-11-11 | 2021-01-05 | 苏州鑫极纺织有限公司 | Skin-core structure water-absorbing fiber and preparation method thereof |
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