CN114606591A - anti-UV (ultraviolet) regenerated polyester chip and preparation method and application thereof - Google Patents
anti-UV (ultraviolet) regenerated polyester chip and preparation method and application thereof Download PDFInfo
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- CN114606591A CN114606591A CN202210337527.8A CN202210337527A CN114606591A CN 114606591 A CN114606591 A CN 114606591A CN 202210337527 A CN202210337527 A CN 202210337527A CN 114606591 A CN114606591 A CN 114606591A
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- 229920000728 polyester Polymers 0.000 title claims abstract description 63
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 239000000843 powder Substances 0.000 claims abstract description 54
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 45
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims abstract description 30
- 239000002131 composite material Substances 0.000 claims abstract description 25
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 22
- 239000004744 fabric Substances 0.000 claims abstract description 14
- 238000002844 melting Methods 0.000 claims abstract description 13
- 230000008018 melting Effects 0.000 claims abstract description 13
- 239000000835 fiber Substances 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims description 33
- 238000002156 mixing Methods 0.000 claims description 27
- 239000000654 additive Substances 0.000 claims description 24
- 230000000996 additive effect Effects 0.000 claims description 24
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 17
- 238000001035 drying Methods 0.000 claims description 15
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 14
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 14
- 239000002994 raw material Substances 0.000 claims description 10
- 239000002270 dispersing agent Substances 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 8
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims description 7
- ZMZNLKYXLARXFY-UHFFFAOYSA-H cerium(3+);oxalate Chemical compound [Ce+3].[Ce+3].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O ZMZNLKYXLARXFY-UHFFFAOYSA-H 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 238000010304 firing Methods 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 235000006408 oxalic acid Nutrition 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- RKISUIUJZGSLEV-UHFFFAOYSA-N n-[2-(octadecanoylamino)ethyl]octadecanamide Chemical compound CCCCCCCCCCCCCCCCCC(=O)NCCNC(=O)CCCCCCCCCCCCCCCCC RKISUIUJZGSLEV-UHFFFAOYSA-N 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 229960001759 cerium oxalate Drugs 0.000 claims description 3
- VYLVYHXQOHJDJL-UHFFFAOYSA-K cerium trichloride Chemical compound Cl[Ce](Cl)Cl VYLVYHXQOHJDJL-UHFFFAOYSA-K 0.000 claims description 3
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 3
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 3
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 3
- 150000002148 esters Chemical class 0.000 claims description 2
- 230000005855 radiation Effects 0.000 abstract description 4
- 238000011161 development Methods 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 238000007380 fibre production Methods 0.000 abstract description 2
- 229920000139 polyethylene terephthalate Polymers 0.000 description 39
- 239000005020 polyethylene terephthalate Substances 0.000 description 39
- 230000008569 process Effects 0.000 description 10
- 238000009987 spinning Methods 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 9
- 239000004753 textile Substances 0.000 description 7
- 239000002699 waste material Substances 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 239000011248 coating agent Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 238000009941 weaving Methods 0.000 description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 4
- 230000006750 UV protection Effects 0.000 description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- WOZVHXUHUFLZGK-UHFFFAOYSA-N dimethyl terephthalate Chemical compound COC(=O)C1=CC=C(C(=O)OC)C=C1 WOZVHXUHUFLZGK-UHFFFAOYSA-N 0.000 description 4
- 238000001125 extrusion Methods 0.000 description 4
- 230000004224 protection Effects 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- -1 Polyethylene terephthalate Polymers 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 208000000453 Skin Neoplasms Diseases 0.000 description 1
- 230000004931 aggregating effect Effects 0.000 description 1
- 125000005250 alkyl acrylate group Chemical group 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 235000013361 beverage Nutrition 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 229940044927 ceric oxide Drugs 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 238000007720 emulsion polymerization reaction Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 239000010954 inorganic particle Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 201000000849 skin cancer Diseases 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 229920006337 unsaturated polyester resin Polymers 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/106—Radiation shielding agents, e.g. absorbing, reflecting agents
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Artificial Filaments (AREA)
Abstract
The invention belongs to the technical field of functional fiber production, and particularly relates to an anti-UV (ultraviolet) regenerated polyester chip and a preparation method and application thereof. According to the preparation method, the cerium dioxide and titanium dioxide composite powder is added into the recovered PET powder in an online melting and adding manner, so that the regenerated polyester chip with excellent ultraviolet radiation resistance is prepared, has the characteristics of uniform and rich color, high color fastness, good spinnability and the like, can be applied to preparation of fibers or fabrics, and develops development and utilization of the cerium dioxide in the field of chemical fibers.
Description
Technical Field
The invention belongs to the technical field of functional fiber production, and particularly relates to an anti-UV (ultraviolet) regenerated polyester chip and a preparation method and application thereof.
Background
Polyethylene terephthalate (PET) is a saturated high molecular compound obtained by Polycondensation of Terephthalic Acid (PTA) or dimethyl terephthalate (DMT) and ethylene glycol, belongs to a crystalline high polymer, and is widely used in bottles such as beverage bottles. The bottle bodies can be recycled after being used up, and the recycled PET bottle chips are mainly used for manufacturing fibers, sheets, non-food packaging bottles and unsaturated polyester resins. Currently, worldwide polyester production is on the order of several million tons per year, while its consumption is still increasing at a rate of 11% per year. If the used waste polyester is directly discharged into the environment, the environment is polluted and resources are wasted. Therefore, the recycling of PET polyester has great significance for protecting the environment and relieving the world resource crisis, the recycling of waste polyester products can change waste into valuable, the pressure of the shortage of non-renewable resources such as petroleum and the like is relieved, and meanwhile, the recycling of PET polyester has great significance for protecting the ecological environment, the sustainable development of the polyester industry and the like.
Meanwhile, with the damage of human activities to the atmospheric ozone layer, ultraviolet radiation has become one of the great threats to human health, and the probability of human skin cancer is increased. Nowadays, the sales of ultraviolet-resistant cosmetics and daily necessities are increased rapidly, but the protection capability, the protection area and the action time are limited. Therefore, the textile with larger area and better protection effect is used for blocking the excessive damage of ultraviolet rays to human bodies, becomes a barrier for protecting the skin from the ultraviolet rays, and becomes an important direction.
At present, in the production of ultraviolet-proof textiles at home and abroad, an ultraviolet screening agent is generally used for dipping or coating on the surface of the textile to play a role in protection; or adding ultraviolet screening agent during polymerization or spinning. Patent CN200958152Y discloses a method for preparing an anti-ultraviolet towel, which uses towel yarn containing nano ZnO or TiO2The finishing agent is obtained by dipping treatment, and the method has simple process and poor durability. Patent application CN107936201A proposes an ultraviolet-resistant coating fabric, which comprises a fabric base material and an ultraviolet-resistant coating agent coated on the base material, wherein the ultraviolet-resistant coating agent is prepared by emulsion polymerization of deionized water, an emulsifier, alkyl acrylate, alkyl methacrylate, an aryl unsaturated monomer, a crosslinking monomer, a coupling agent, nano titanium dioxide and other components under the action of an initiator. Although the fabric in the scheme has a certain ultraviolet-resistant effect, the color fastness of the coating on the surface of the fabric is poor and the coating is easy to fall off, so that the using effect of the fabric is influenced.
At present, common recycled polyester chips do not have the ultraviolet protection effect. Therefore, the waste PET is recycled and prepared into the anti-UV recycled polyester chip, so that the environment is protected, the application range of the recycled polyester chip in the textile can be expanded, and the additional value of the textile is improved.
Disclosure of Invention
Therefore, the anti-UV regenerated polyester chip and the preparation method and application thereof are needed to be provided, the cerium dioxide and titanium dioxide composite powder is added into the recycled PET powder in an online melting and adding mode, the preparation process is simple, and the prepared regenerated polyester chip has excellent anti-ultraviolet radiation performance and good spinnability.
In order to achieve the purpose, the invention adopts the main technical scheme that:
in a first aspect, the invention provides a preparation method of an anti-UV recycled polyester chip, which comprises the following steps:
mixing cerium dioxide powder and titanium dioxide powder, and drying to obtain a composite additive for later use;
fully mixing the recovered PET powder with the composite additive to obtain a mixed material;
and automatically metering the mixed material and the recycled PET polyester, adding the mixed material and the recycled PET polyester into a double-screw extruder, and melting, extruding, water-cooling, bracing and dicing to obtain the anti-UV regenerated polyester chip.
In a further embodiment of the present invention, the cerium oxide and the titanium dioxide powder are mixed at a mass ratio of 1:1 to 9: 1. Wherein 1:1 to 9:1 can also be represented as 1 to 9: 1.
In a further embodiment of the present invention, the mixing mass ratio of the recycled PET powder to the composite additive is 1:1 to 4: 1. Wherein 1:1 to 4:1 can also be expressed as 1 to 4: 1.
As a further embodiment of the invention, the amount of the mixed material is 1 to 3 percent of the mass of the recycled PET polyester.
In a further embodiment of the present invention, a dispersant is further added to the mixture, wherein the dispersant is a mixture of one or more of a modified ester dispersant, EBS (N, N' -ethylene bis stearamide), and polyvinylpyrrolidone. The dispersant can prevent titanium dioxide and cerium oxide from aggregating in the polyester, thereby increasing dispersibility.
Preferably, the dosage of the dispersant is 1 to 5 percent of the mass of the composite additive.
As a further embodiment of the present invention, the preparation of the cerium oxide powder includes the steps of:
taking cerium chloride or cerium nitrate as a raw material, adjusting the pH value to 2-4, adding oxalic acid to precipitate cerium oxalate, heating, curing, separating, washing, drying, and firing at 900-1000 ℃ to obtain cerium dioxide;
and grinding the cerium dioxide to obtain the cerium dioxide powder.
As a further embodiment of the present invention, the cerium oxide powder has a particle size of less than 0.1 μm. By controlling the particle size of the cerium dioxide powder to be less than 0.1 mu m, the dispersibility of the cerium dioxide powder is further enhanced, and the phenomenon that inorganic particles are easy to agglomerate can be overcome in the blending synergistic effect with titanium dioxide and the blending process with recycled PET powder. When the particle size of the cerium dioxide powder is larger than 0.1 mu m, agglomeration is easy to occur in the subsequent blending process, the spinnability is poor in the spinning process, and the filaments and the ends are easy to fly.
As a further embodiment of the present invention, the moisture content of the composite additive is less than 100 ppm. The moisture content of the composite additive is controlled to be less than 100ppm, so that the degradation of PET in the adding process is avoided, the viscosity is reduced, and the physical indexes of the fabric are influenced.
In a second aspect, the invention provides an anti-UV recycled polyester chip, which is prepared by the preparation method of the first aspect of the invention.
In a third aspect, the present invention provides the use of the UV resistant recycled polyester chip of the first aspect of the present invention in the preparation of a fiber or fabric.
Different from the prior art, the technical scheme adds the cerium dioxide and titanium dioxide composite powder into the recovered PET powder in an online melting adding mode to prepare the regenerated polyester chip with excellent ultraviolet radiation resistance, has the characteristics of uniform and rich color, high color fastness, good spinnability and the like, is green and clean, can be recycled, and develops the development and utilization of the cerium dioxide in the field of chemical fibers.
Detailed Description
In order to explain technical contents, structural features, and objects and effects of the technical means in detail, the following detailed description is given with reference to specific embodiments.
In the description of this application, a numerical range denoted by "value a to value B" is intended to include the endpoint value A, B, and all integers and fractions within the range. For example, "1: 1-4: 1" refers to "1-4: 1" and includes, but is not limited to, 1:1, 1.5:1, 2:1, 2.5:1, 3:1, 4:1, and the like.
In the present application, when an equivalent, concentration, or other value or parameter is expressed as a range, preferred range, or as a range defined by a list of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed.
The term "prepared from …" as used herein is synonymous with "comprising". The terms "comprises," "comprising," "includes," "including," "has," "having," "contains," "containing," or any other variation thereof, as used herein, are intended to cover a non-exclusive inclusion. For example, a composition, process, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, process, method, article, or apparatus.
Approximating language, as used herein in the specification and claims, is intended to modify a quantity, such that the invention is not limited to the specific quantity, but includes portions that are literally equivalent to the specific quantity, subject to modification without resulting in a change in the basic function to which it is related. Accordingly, the use of "about" to modify a numerical value means that the invention is not limited to the precise value. In some instances, the approximating language may correspond to the precision of a numerical value.
The indefinite articles "a" and "an" preceding an element or component of the present application do not limit the quantitative requirement (i.e., the number of occurrences) of the element or component. Thus, "a" or "an" should be read to include one or at least one, and the singular form of an element or component also includes the plural unless the stated number clearly indicates that the singular form is intended.
Furthermore, unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In case of conflict, the present specification, including definitions, will control.
Test materials, reagents and the like used in the following examples are commercially available unless otherwise specified. The experimental procedures in the following examples are conventional unless otherwise specified.
In the specific embodiment of the application, the recovered PET powder is prepared by recovering and cleaning waste PET bottle flakes, crushing the waste PET bottle flakes into powder, and drying the powder; the recovered PET polyester is obtained by recovering, cleaning and drying the waste PET bottle chips.
In the specific embodiment of the present application, the titanium dioxide powder is a nano titanium dioxide powder, and is commercially available.
Example 1 preparation and application of anti-UV recycled polyester chip
Using cerium chloride as a raw material, adjusting the pH value to 2 by using ammonia water, adding oxalic acid to precipitate cerium oxalate, heating, curing, separating, washing, drying at 110 ℃, and then firing at 900 ℃ to prepare cerium dioxide;
grinding cerium dioxide to make its grain size be up to 0.1 micrometer;
mixing cerium dioxide powder and titanium dioxide powder according to the proportion of 1:1, and drying until the moisture content reaches below 100ppm to obtain the composite additive for later use;
mixing the recovered PET powder with a composite additive according to the weight ratio of 1:1, fully mixing in a high-speed mixer to obtain a mixed material, so that the mixed material is convenient for on-line melting and adding;
and (3) automatically metering and adding the mixed material and the recycled PET into a double-screw extruder through a full-automatic feeding machine, and carrying out melting, extrusion, water cooling, bracing and dicing to obtain the recycled polyester chips. Wherein, the mixed materials are automatically metered and added through a side feeding port; the recycled PET polyester is automatically metered and added through the main feeding port. The amount of the mixed material was 1 wt% (including 0.5 wt% of titanium dioxide and 0.5 wt% of cerium oxide) in terms of the mass percentage of the recycled PET polyester.
And spinning and weaving the regenerated polyester chips to respectively obtain polyester fibers (spun yarns) and functional polyester fabrics. The spinning equipment and the weaving equipment are conventional equipment in the field of textile, and working parameters of the spinning equipment and the weaving equipment can also be set according to a conventional method, which is not specifically discussed in the specific embodiment of the application.
Example 2 preparation and application of anti-UV recycled polyester chip
Using cerous nitrate as raw material, regulating pH value to 2 with ammonia water, adding oxalic acid to precipitate cerous oxalate, heating for curing, separating, washing, drying at 105 deg.C, and firing at 1000 deg.C to obtain ceric oxide;
grinding cerium dioxide to make its grain size be up to 0.1 micrometer;
mixing cerium dioxide powder and titanium dioxide powder according to the weight ratio of 9:1, and drying until the moisture content reaches below 100ppm to obtain the composite additive for later use;
mixing the recovered PET powder with a composite additive according to a ratio of 4:1, fully mixing in a high-speed mixer, and simultaneously adding polyvinylpyrrolidone accounting for 1% of the mass of the composite additive to obtain a mixed material, so that the mixed material is convenient for on-line melting and adding;
and (3) automatically metering and adding the mixed material and the recycled PET into a double-screw extruder through a full-automatic feeding machine, and carrying out melting, extrusion, water cooling, bracing and dicing to obtain the recycled polyester chips. Wherein, the mixed materials are automatically metered and added through a side feeding port; the recycled PET polyester is automatically metered and added through the main feeding port. The amount of the mixed material was 2 wt% (including 0.2 wt% titanium dioxide and 1.8 wt% cerium oxide) in terms of the mass percentage of the recycled PET polyester.
And spinning and weaving the regenerated polyester chips to respectively obtain polyester fibers (spun yarns) and functional polyester fabrics.
Example 3 preparation and application of anti-UV recycled polyester chip
Using cerous nitrate as a raw material, adjusting the pH value to 3 by using ammonia water, adding oxalic acid to precipitate cerous oxalate, heating, curing, separating, washing, drying at 115 ℃, and then firing at 950 ℃ to prepare cerium dioxide;
grinding cerium dioxide to make its grain size be up to 0.1 micrometer;
mixing cerium dioxide powder and titanium dioxide powder according to the ratio of 5:1, and drying until the moisture content reaches below 100ppm to obtain the composite additive for later use;
mixing the recovered PET powder with a composite additive according to the weight ratio of 3:1, fully mixing in a high-speed mixer to obtain a mixed material, so that the mixed material is convenient for on-line melting and adding;
and (3) automatically metering and adding the mixed material and the recycled PET into a double-screw extruder through a full-automatic feeding machine, and carrying out melting, extrusion, water cooling, bracing and dicing to obtain the recycled polyester chips. Wherein, the mixed materials are automatically metered and added through a side feeding port; the recycled PET polyester is automatically metered and added through the main feeding port. The amount of the mixed material was 3 wt% (including 0.5 wt% titanium dioxide and 2.5 wt% cerium oxide) in terms of the mass percentage of the recycled PET polyester.
And spinning and weaving the regenerated polyester chips to respectively obtain polyester fibers (spun yarns) and functional polyester fabrics.
Example 4 preparation and application of anti-UV recycled polyester chip
Using cerous nitrate as a raw material, adjusting the pH value to 4 by using ammonia water, adding oxalic acid to precipitate cerous oxalate, heating, curing, separating, washing, drying at 110 ℃, and then firing at 980 ℃ to prepare cerium dioxide;
grinding cerium dioxide to make its grain size be up to 0.1 micrometer;
mixing cerium dioxide powder and titanium dioxide powder according to the weight ratio of 7: 1, and drying until the moisture content reaches below 100ppm to obtain the composite additive for later use;
mixing the recovered PET powder with a composite additive according to the weight ratio of 2:1, fully mixing in a high-speed mixer, and simultaneously adding EBS accounting for 3% of the mass of the composite additive to obtain a mixed material, so that the mixed material is convenient for on-line melting and adding;
and (3) automatically metering and adding the mixed material and the recycled PET into a double-screw extruder through a full-automatic feeding machine, and carrying out melting, extrusion, water cooling, bracing and dicing to obtain the recycled polyester chips. Wherein, the mixed materials are automatically metered and added through a side feeding port; the recycled PET polyester is automatically metered and added through the main feeding port. The amount of the mixed material was 1.6 wt% (including 0.2 wt% titanium dioxide and 1.4 wt% cerium oxide) in terms of the mass percentage of the recycled PET polyester.
And spinning and weaving the regenerated polyester chips to respectively obtain polyester fibers (spun yarns) and functional polyester fabrics.
Comparative example 1
The raw materials, the amounts and the preparation methods of this comparative example were the same as those of example 1, except that ceria was ground to have a particle size of about 0.15 μm. The cerium dioxide powder has poor dispersibility, and is easy to agglomerate in the blending synergistic effect with the titanium dioxide powder and the blending process with the PET powder; in the spinning process, the ends are easily broken.
Comparative example 2
The comparative example was prepared using the same raw materials, amounts and preparation method as example 1, except that the water content of the composite additive was about 200ppm after drying. Agglomeration easily occurs during blending of cerium oxide powder with titanium dioxide powder and blending with PET powder.
Comparative example 3
In the comparative example, cerium oxide powder was not added, and only titanium dioxide powder was used as an additive; the mass ratio of the titanium dioxide powder to the recycled PET powder is not less than 1: 1. the rest raw materials, the dosage and the process method are the same as those of the example 1.
Comparative example 4
The raw materials, the amounts, and the preparation methods of the present comparative example were the same as those of example 1, except that cerium oxide was ground to have a particle size of about 0.20 μm and the moisture content of the composite additive was about 200 ppm. In the process of blending materials, the agglomeration phenomenon is most obvious, and in the spinning process, the end breakage is easy, and the operation difficulty is large.
Examples of the experiments
The polyester fibers and the polyester fabrics provided in examples 1 to 4 and comparative examples 1 to 4 were subjected to performance tests, and the test results are shown in table 1.
(1) Testing the breaking strength and the breaking elongation by adopting a GB/T14344-2008 chemical fiber filament tensile property test method;
(2) according to GB/T18830-2009-evaluation standards of ultraviolet resistance performance of textiles, 5 points are taken at different positions of each sample, the transmittance (UVA and UVB) of the sample to ultraviolet light with the wavelength of 200-400 nm and an ultraviolet resistance coefficient UPF are tested, and the average value is taken; washing with clean water with the same parameters for 100 times, comparing the ultraviolet transmittance (UVA, UVB) and ultraviolet protection coefficient (UPF) of each group after washing, taking 5 points at different positions for testing, and taking an average value.
Table 1:
it should be noted that, although the above embodiments have been described herein, the scope of the present invention is not limited thereby. Therefore, based on the innovative concepts of the present invention, the technical solutions of the present invention can be directly or indirectly applied to other related technical fields by making changes and modifications to the embodiments described herein or by using equivalent structures or equivalent processes performed in the present specification, and are included in the scope of the present invention.
Claims (10)
1. The preparation method of the anti-UV recycled polyester chip is characterized by comprising the following steps:
mixing cerium dioxide powder and titanium dioxide powder, and drying to obtain a composite additive for later use;
fully mixing the recovered PET powder with the composite additive to obtain a mixed material;
and automatically metering the mixed material and the recycled PET polyester, adding the mixed material and the recycled PET polyester into a double-screw extruder, and melting, extruding, water-cooling, bracing and dicing to obtain the anti-UV regenerated polyester chip.
2. The production method according to claim 1, wherein the mixing mass ratio of the cerium oxide powder to the titanium dioxide powder is 1:1 to 9: 1.
3. The preparation method according to claim 1, wherein the mixing mass ratio of the recycled PET powder to the composite additive is 1: 1-4: 1.
4. The preparation method according to claim 1, wherein the amount of the mixed material is 1 to 3% of the mass of the recycled PET polyester.
5. The preparation method according to claim 4, characterized in that a dispersant is further added into the mixed material, wherein the dispersant is a mixture of one or more of modified ester dispersant, EBS (N, N' -ethylene bis stearamide) and polyvinylpyrrolidone;
preferably, the dosage of the dispersant is 1 to 5 percent of the mass of the composite additive.
6. The preparation method according to claim 1, wherein the preparation of the cerium oxide powder comprises the steps of:
taking cerium chloride or cerium nitrate as a raw material, adjusting the pH value to 2-4, adding oxalic acid to precipitate cerium oxalate, heating, curing, separating, washing, drying, and firing at 900-1000 ℃ to obtain cerium dioxide;
and grinding the cerium dioxide to obtain the cerium dioxide powder.
7. The method of claim 1, wherein the cerium oxide powder has a particle size of less than 0.1 μm.
8. The method of claim 1, wherein the moisture content of the additive package is less than 100 ppm.
9. An anti-UV recycled polyester chip, which is prepared by the preparation method of any one of claims 1 to 8.
10. Use of the UV resistant recycled polyester chip of claim 9 for the preparation of fibers or fabrics.
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