CN104911746B - A kind of polyester fiber with energy-saving and temperature-regulating function and preparation method thereof - Google Patents
A kind of polyester fiber with energy-saving and temperature-regulating function and preparation method thereof Download PDFInfo
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- CN104911746B CN104911746B CN201510299141.2A CN201510299141A CN104911746B CN 104911746 B CN104911746 B CN 104911746B CN 201510299141 A CN201510299141 A CN 201510299141A CN 104911746 B CN104911746 B CN 104911746B
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Abstract
The invention provides a kind of polyester fiber with energy-saving and temperature-regulating function, it is characterized in that, including Part I and Part II, described Part II is inside Part I, raw material of the described Part I including comprising spinning grade polyester is made, raw material of the described Part II including comprising matrix polymer, phase change medium, foaming agent azodicarbonamide, activator and assistant crosslinking agent is made, described Part II has hole-closing structure, and described phase change medium is distributed in hole-closing structure between hole-closing structure.The polyester fiber of energy-saving and temperature-regulating function prepared by the present invention has imitation leather cored structure or a double structure separation structures, and its sandwich layer or fibril have a uniform hole-closing structure, and phase transformation medium storing is in closed pore space or being embedded in the middle of hole wall.Closed pore in the structure both can seal air up for safekeeping again with grappling phase change medium, reach the effect of insulation cooperative effect.
Description
Technical field
The invention belongs to the preparation field of intelligent temperature adjusting fiber, more particularly to a kind of polyester with energy-saving and temperature-regulating function is fine
Dimension and preparation method thereof.
Background technology
With the continuing to develop of social demand, the increasingly change of living environment, people are to taking and household textiles is proposed
The demand of multifunctional intelligent.In terms of the comfortableness that skin is contacted, human body warm is particularly important.Warming-type intelligent thermoregulating is fine
Dimension can be using fiber itself is to the storage of heat and discharges to reach the purpose of microenvironment between regulation human body and fabric.Polyester is fine
Dimension is as current topmost textile raw material, and the polyester production capacity of China's Mainland in 2013 reaches 31,000,000 tons, in functionalized polyester
Market is very wide in terms of fiber, but the product marketization of industrialization and performance stabilization is seldom.
The preparation method of current thermo-regulated fiber has microcapsules wet spinning process, doughnut completion method, fiber surface
Completion method etc..There is preparation process pollution greatly in microcapsules wet spinning process, the drawbacks of process is numerous and diverse；Doughnut completion method,
Have the shortcomings that phase-change material is easily revealed；There is the defect of washability difference in fiber surface coating.Patent of invention CN
Doughnut is put into hopper by 103710964 A, carries out the filling of phase-change material, the end-blocking of its fiber ends has problem.
The B of patent of invention CN 101906670 disclose spinning equipment and its preparation side of a kind of melt-spun type solid-liquid composite phase change fiber
Method, is directly stored in fibrous inside, there is also shakiness for liquid state phase change material fusingization in liquid form by liquid state phase change material
The problem of determining.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of polyester fiber with energy-saving and temperature-regulating function and its preparation
Method, fibre section prepared by this method is rendered as imitation leather cored structure or double structure separation structures, and its sandwich layer or fibril, which have, uniformly to be closed
Pore structure, phase transformation medium storing is in closed pore space or being embedded in the middle of hole wall.The Intelligent energy storage temperature-regulating fiber tool of the present invention
Have the advantages that cost is low, polluting small, enthalpy, high, energy-saving and temperature-regulating ability is strong, can preferably apply the functionalization in polyester fiber to change
Property field, meets chemical fibre industry production requirement.
In order to solve the above-mentioned technical problem, the invention provides a kind of polyester fiber with energy-saving and temperature-regulating function, it is special
Levy and be, including Part I and Part II, described Part II inside Part I, described Part I by
It is made comprising the raw material including spinning grade polyester, described Part II is by even comprising matrix polymer, phase change medium, foaming agent
Raw material including nitrogen diformamide, activator and assistant crosslinking agent is made, and described Part II has hole-closing structure, institute
The phase change medium stated is distributed in hole-closing structure between hole-closing structure.
Preferably, it is cortex that described Part I and Part II, which constitute Part I, and Part II is the skin of sandwich layer
Cored structure constitutes double structure separation structures that Part II is dispersed in inside Part I.
Preferably, described spinning grade polyester is polyethylene terephthalate, PTT, gathered
Mutual-phenenyl two acid bromide two alcohol ester or PEN.
Preferably, described matrix polymer is polyethylene terephthalate, PTT, gathered
Mutual-phenenyl two acid bromide two alcohol ester, polypropylene, makrolon, polyurethane or polyethylene.
Preferably, the melting temperature of described matrix polymer at one atm is 90~130 DEG C.
Preferably, described phase change medium is polyethylene glycol, paraffin, stearic acid, laurate, SA, polyethyleneglycol
One or more in acrylate, stearyl chloride, lauroyl chloride and certain herbaceous plants with big flowers diacid chloride.
Preferably, described assistant crosslinking agent is cumyl peroxide or di-tert-butyl peroxide.
Preferably, the mass ratio of described Part I and Part II is 1/3~9/1.
Preferably, described Part II by 20~60wt% of phase change medium, foaming agent azodicarbonamide 0.5~5%,
The matrix polymer of activator 0.5~1%, assistant crosslinking agent 0.2~1% and surplus is made.
Preferably, the hole ratio of the hole-closing structure of described Part II is 20~50%, and aperture is 0.1~1 μm.
Present invention also offers the preparation method of the above-mentioned polyester fiber with energy-saving and temperature-regulating function, it is characterised in that
Specific steps include：The raw material of the raw material of Part I and Part II is added into the composite spinning system with two single screw rods
System, carries out melt spinning using bicomponent fibre component or double structures point fiber sprinning assembly, obtains with energy-saving and temperature-regulating function
Polyester fiber.
The present invention utilizes sandwich layer or fibrillar structure using the method for imitation leather cored structure bicomponent fibre or double structures point fiber
In uniform hole-closing structure, phase transformation medium is sealed up for safekeeping, and partial phase change material can be directly embedded in the middle of hole wall.
Compared with prior art, the beneficial effects of the invention are as follows：
(1) polyester fiber of energy-saving and temperature-regulating function prepared by the present invention has imitation leather cored structure or double structure separation structures, its core
Layer or fibril have a uniform hole-closing structure, and phase transformation medium storing is in closed pore space or being embedded in the middle of hole wall.In the structure
Closed pore both can seal air up for safekeeping again with grappling phase change medium, reach the effect of insulation cooperative effect.
(2) polyester fiber of energy-saving and temperature-regulating function of the invention have that cost is low, high, the energy-saving and temperature-regulating energy that pollutes small, enthalpy
The strong advantage of power, can preferably apply in the functional modification field of polyester fiber, meet chemical fibre industry production requirement.
Brief description of the drawings
Fig. 1 a are the polyester fiber structures schematic diagram with energy-saving and temperature-regulating function of imitation leather cored structure
Fig. 1 b are the polyester fiber sectional view with energy-saving and temperature-regulating function of imitation leather cored structure；
Fig. 2 a are the polyester fiber structures schematic diagram with energy-saving and temperature-regulating function of double structure separation structures
Fig. 2 b are the polyester fiber sectional view with energy-saving and temperature-regulating function of double structure separation structures；
In figure, 1 is Part I, and 2 be Part II, and 3 be phase change medium.
Embodiment
With reference to specific embodiment, the present invention is expanded on further.It should be understood that these embodiments are merely to illustrate the present invention
Rather than limitation the scope of the present invention.In addition, it is to be understood that after the content of the invention lectured has been read, people in the art
Member can make various changes or modifications to the present invention, and these equivalent form of values equally fall within the application appended claims and limited
Scope.Polyethylene glycol monoacrylate described in various embodiments of the present invention is closed with reference to the B of national inventing patent CN 102516471
Into its number-average molecular weight is 1000~10000.Phase transformation enthalpy in various embodiments of the present invention is determined by DSC to be obtained.
Embodiment 1
As seen in figure la and lb, a kind of polyester fiber with energy-saving and temperature-regulating function, by Part I 1 and Part II 2
Composition, described Part II 2 is inside Part I 1, and described Part I 1 is made up of spinning grade polyester, described
Part II 2 is made up of matrix polymer, phase change medium, foaming agent azodicarbonamide, activator and assistant crosslinking agent,
Described Part II 2 has hole-closing structure, and phase change medium 3 is distributed in hole-closing structure between hole-closing structure.
It is cortex that described Part I and Part II, which constitute Part I, and Part II is the skin-core structure of sandwich layer.
Described spinning grade polyester is polyethylene terephthalate.Described matrix polymer is fusing point at one atm
Temperature is 130 DEG C of polyethylene terephthalate.Described phase change medium is polyethylene glycol monoacrylate.Described helps
Crosslinking agent is cumyl peroxide.
The preparation method of the above-mentioned polyester fiber with energy-saving and temperature-regulating function is：First, with two single screw rods
50 parts by weight poliester chips are added in first single screw rod of composite spinning system, with two single spiral shells
Second single screw rod of the composite spinning system of bar adds polyethylene glycol monoacrylate, the azo of 2.5 parts by weight of 30 parts by weight
Diformamide, the nano zine oxide (50~200nm of particle diameter) of 0.5 parts by weight, the cumyl peroxide of 0.5 parts by weight, 16.5
The fusing point of parts by weight is the pre-composition of 130 DEG C of polyethylene terephthalates, and the head pressure of its second single screw rod compares first
High 0.5~the 1MPa of head pressure of single screw rod.Then the bi-component sheath-core of the composite spinning system with two single screw rods is utilized
Filament spinning component melt spinning, spinning temperature is 270 DEG C, and spinning speed is 1500m/min, obtains poly- with energy-saving and temperature-regulating function
Ester fiber, its center core layer hole ratio is about 50% and aperture is about 1 μm of uniform hole-closing structure.Experiment is found, prepares fiber
Phase transformation enthalpy reaches 20~30J/g.
Embodiment 2
As seen in figure la and lb, a kind of polyester fiber with energy-saving and temperature-regulating function, by Part I 1 and Part II 2
Composition, described Part II 2 is inside Part I 1, and described Part I 1 is made up of spinning grade polyester, described
Part II 2 is made up of matrix polymer, phase change medium, foaming agent azodicarbonamide, activator and assistant crosslinking agent,
Described Part II 2 has hole-closing structure, and phase change medium 3 is distributed in hole-closing structure between hole-closing structure.
It is cortex that described Part I and Part II, which constitute Part I, and Part II is the skin-core structure of sandwich layer.
Described spinning grade polyester is polyethylene terephthalate.Described matrix polymer is fusing point at one atm
Temperature is 130 DEG C of polyethylene terephthalate.Described phase change medium is polyethylene glycol and SA.Described helps friendship
Connection agent is di-tert-butyl peroxide.
The preparation method of the above-mentioned polyester fiber with energy-saving and temperature-regulating function is：First, with two single screw rods
The section of 50 parts by weight PTTs is added in first single screw rod of composite spinning system, with two single spiral shells
Polyethylene glycol (number-average molecular weight is 2000), 15 weight of 15 parts by weight are added in second single screw rod of the composite spinning system of bar
SA, the azodicarbonamide of 2.5 parts by weight, the nano zine oxide (50~200nm of particle diameter), 0.5 weight of 0.5 parts by weight of part
The pre-composition of the di-tert-butyl peroxide of part, the fusing point of 16.5 parts by weight for 130 DEG C of polyethylene terephthalates is measured, its
In the second single screw rod head pressure high 0.5~1MPa of the head pressure than the first single screw rod.Then using with two single spiral shells
The bi-component sheath-core filament spinning component melt spinning of the composite spinning system of bar, spinning temperature is 270 DEG C, and spinning speed is 800m/
Min, obtains the polyester fiber with energy-saving and temperature-regulating function, and its center core layer hole ratio is about 20% and aperture is about 0.1 μm equal
Even hole-closing structure.Experiment finds that the phase transformation enthalpy for preparing fiber reaches 10~20J/g.
Embodiment 3
As shown in figures 2 a and 2b, a kind of polyester fiber with energy-saving and temperature-regulating function, by Part I 1 and Part II 2
Composition, described Part II 2 is inside Part I 1, and described Part I 1 is made up of spinning grade polyester, described
Part II 2 is made up of matrix polymer, phase change medium, foaming agent azodicarbonamide, activator and assistant crosslinking agent,
Described Part II 2 has hole-closing structure, and phase change medium 3 is distributed in hole-closing structure between hole-closing structure.
Described Part I and Part II constitute double structure separation structures that Part II is dispersed in inside Part I.Institute
The spinning grade polyester stated is polyethylene terephthalate.Described matrix polymer is fusing point temperature at one atm
Spend for 90 DEG C of polyethylene.Described phase change medium is paraffin.Described assistant crosslinking agent is cumyl peroxide.
The preparation method of the above-mentioned polyester fiber with energy-saving and temperature-regulating function is：First, with two single screw rods
The section of 90 parts by weight polybutylene terephthalate (PBT)s is added in first single screw rod of composite spinning system, with two single spiral shells
The paraffin of 2 parts by weight, the azodicarbonamide of 0.05 parts by weight, 0.05 are added in second single screw rod of the composite spinning system of bar
Nano zine oxide (50~200nm of particle diameter), the cumyl peroxide of 0.02 parts by weight, the fusing point of 7.88 parts by weight of parts by weight
The pre-composition cut into slices for 90 DEG C of polyethylene, wherein the head pressure of the second single screw rod is higher than the head pressure of the first single screw rod by 0.5
~1MPa.Then double structures point filament spinning component melt spinning of the composite spinning system with two single screw rods, spinning temperature are utilized
For 250 DEG C, spinning speed is 1000m/min, obtains the hole of the polyester fiber with energy-saving and temperature-regulating function, wherein class fibrillar structure
Hole rate is about 50% and aperture is about 1 μm of uniform hole-closing structure.Experiment finds, the phase transformation enthalpy for preparing fiber reaches 2~
5J/g。
Embodiment 4
As seen in figure la and lb, a kind of polyester fiber with energy-saving and temperature-regulating function, by Part I 1 and Part II 2
Composition, described Part II 2 is inside Part I 1, and described Part I 1 is made up of spinning grade polyester, described
Part II 2 is made up of matrix polymer, phase change medium, foaming agent azodicarbonamide, activator and assistant crosslinking agent,
Described Part II 2 has hole-closing structure, and phase change medium 3 is distributed in hole-closing structure between hole-closing structure.
It is cortex that described Part I and Part II, which constitute Part I, and Part II is the skin-core structure of sandwich layer.
Described spinning grade polyester is polybutylene terephthalate (PBT).Described matrix polymer is fusing point at one atm
Temperature is 130 DEG C of polypropylene.Described phase change medium is stearic acid.Described assistant crosslinking agent is cumyl peroxide.
The preparation method of the above-mentioned polyester fiber with energy-saving and temperature-regulating function is：First, with two single screw rods
The section of 25 parts by weight polybutylene terephthalate (PBT)s is added in first single screw rod of composite spinning system, with two single spiral shells
Stearic acid, the formyl of azo two of 2.25 parts by weight of 22.5 parts by weight are added in second single screw rod of the composite spinning system of bar
Nano zine oxide (50~200nm of particle diameter), the cumyl peroxide of 0.375 parts by weight, 49.125 weights of amine, 0.75 parts by weight
It is 130 DEG C of polyacrylic pre-compositions to measure the fusing point of part, wherein head pressure of the head pressure of the second single screw rod than the first single screw rod
High 0.5~the 1MPa of power.Then spun using the bi-component sheath-core filament spinning component melting of the composite spinning system with two single screw rods
Silk, spinning temperature is 280 DEG C, and spinning speed is 2000m/min, obtains the polyester fiber with energy-saving and temperature-regulating function, its SMIS
Layer hole ratio is about 30% and aperture is about 0.5 μm of uniform hole-closing structure.Experiment finds that the phase transformation enthalpy for preparing fiber reaches
To 20~30J/g.
Embodiment 5
As seen in figure la and lb, a kind of polyester fiber with energy-saving and temperature-regulating function, by Part I 1 and Part II 2
Composition, described Part II 2 is inside Part I 1, and described Part I 1 is made up of spinning grade polyester, described
Part II 2 is made up of matrix polymer, phase change medium, foaming agent azodicarbonamide, activator and assistant crosslinking agent,
Described Part II 2 has hole-closing structure, and phase change medium 3 is distributed in hole-closing structure between hole-closing structure.
It is cortex that described Part I and Part II, which constitute Part I, and Part II is the skin-core structure of sandwich layer.
Described spinning grade polyester is polyethylene terephthalate.Described matrix polymer is fusing point at one atm
Temperature is 120 DEG C of makrolon.Described phase change medium is stearyl chloride and lauroyl chloride.Described assistant crosslinking agent is peroxide
Change diisopropylbenzene (DIPB).
The preparation method of the above-mentioned polyester fiber with energy-saving and temperature-regulating function is：First, with two single screw rods
50 parts by weight poliester chips are added in first single screw rod of composite spinning system, with two single spiral shells
The stearyl chloride, the lauroyl chloride of 10 parts by weight, 2.5 weights of 20 parts by weight are added in second single screw rod of the composite spinning system of bar
The peroxidating two for measuring the azodicarbonamide, the nano zine oxide (50~200nm of particle diameter) of 0.5 parts by weight, 0.5 parts by weight of part is different
The pre-composition of propyl benzene, the makrolon that the fusing point of 16.5 parts by weight is 120 DEG C, wherein the head pressure of the second single screw rod compares first
High 0.5~the 1MPa of head pressure of single screw rod.Then the bi-component sheath-core of the composite spinning system with two single screw rods is utilized
Filament spinning component melt spinning, spinning temperature is 270 DEG C, and spinning speed is 1000m/min, obtains poly- with energy-saving and temperature-regulating function
Ester fiber, its center core layer hole ratio is about 40% and aperture is about 0.8 μm of uniform hole-closing structure.Experiment is found, prepares fiber
Phase transformation enthalpy reach 8~20J/g.
Embodiment 6
As seen in figure la and lb, a kind of polyester fiber with energy-saving and temperature-regulating function, by Part I 1 and Part II 2
Composition, described Part II 2 is inside Part I 1, and described Part I 1 is made up of spinning grade polyester, described
Part II 2 is made up of matrix polymer, phase change medium, foaming agent azodicarbonamide, activator and assistant crosslinking agent,
Described Part II 2 has hole-closing structure, and phase change medium 3 is distributed in hole-closing structure between hole-closing structure.
It is cortex that described Part I and Part II, which constitute Part I, and Part II is the skin-core structure of sandwich layer.
Described spinning grade polyester is polyethylene terephthalate.Described matrix polymer is fusing point at one atm
Temperature is 95 DEG C of polyurethane.Described phase change medium is certain herbaceous plants with big flowers diacid chloride.Described assistant crosslinking agent is cumyl peroxide.
The preparation method of the above-mentioned polyester fiber with energy-saving and temperature-regulating function is：First, with two single screw rods
50 parts by weight poliester chips are added in first single screw rod of composite spinning system, with two single spiral shells
Added in second single screw rod of the composite spinning system of bar the certain herbaceous plants with big flowers diacid chlorides of 30 parts by weight, the azodicarbonamide of 2.5 parts by weight,
The nano zine oxides (50~200nm of particle diameter) of 0.5 parts by weight, the cumyl peroxide of 0.5 parts by weight, 16.5 parts by weight it is molten
Point for 95 DEG C of polyurethane pre-composition, wherein the head pressure of the second single screw rod it is higher than the head pressure of the first single screw rod by 0.5~
1MPa.Then the bi-component sheath-core filament spinning component melt spinning of the composite spinning system with two single screw rods, spinning temperature are utilized
Spend for 270 DEG C, spinning speed is 2000m/min, obtain the polyester fiber with energy-saving and temperature-regulating function, its center core layer hole ratio is
About 45% and aperture is about 1 μm of uniform hole-closing structure.Experiment finds that the phase transformation enthalpy for preparing fiber reaches 20~30J/g.
Claims (9)
1. a kind of polyester fiber with energy-saving and temperature-regulating function, it is characterised in that described including Part I and Part II
Part II is inside the Part I, and the raw material of described Part I including comprising spinning grade polyester is made, described
Part II by 20 ~ 60wt% of phase change medium, 0.5 ~ 5wt% of foaming agent azodicarbonamide, the wt% of activator 0.5 ~ 1,
0.2 ~ 1wt% of assistant crosslinking agent and the matrix polymer of surplus are made, and described Part II has hole-closing structure, described phase transformation
Dielectric distribution in hole-closing structure between hole-closing structure；The hole ratio of the hole-closing structure of described Part II is 20 ~ 50%,
Aperture is 0.1 ~ 1 μm.
2. have the polyester fiber of energy-saving and temperature-regulating function as claimed in claim 1, it is characterised in that described Part I and
It is cortex that Part II, which constitutes Part I, and Part II is dispersed in first for the skin-core structure or composition Part II of sandwich layer
Double structure separation structures of partial interior.
3. there is the polyester fiber of energy-saving and temperature-regulating function as claimed in claim 1, it is characterised in that described spinning grade polyester
For polyethylene terephthalate, PTT, polybutylene terephthalate (PBT) or poly- naphthalenedicarboxylic acid
Glycol ester.
4. there is the polyester fiber of energy-saving and temperature-regulating function as claimed in claim 1, it is characterised in that described matrix polymer
For polyethylene terephthalate, PTT, polybutylene terephthalate (PBT), polypropylene, poly- carbon
Acid esters, polyurethane or polyethylene.
5. there is the polyester fiber of energy-saving and temperature-regulating function as claimed in claim 1, it is characterised in that described matrix polymer
Melting temperature at one atm is 90 ~ 130oC。
6. there is the polyester fiber of energy-saving and temperature-regulating function as claimed in claim 1, it is characterised in that described phase change medium is
Polyethylene glycol, paraffin, stearic acid, laurate, SA, polyethylene glycol monoacrylate, stearyl chloride, lauroyl chloride and certain herbaceous plants with big flowers two
One or more in acyl chlorides.
7. there is the polyester fiber of energy-saving and temperature-regulating function as claimed in claim 1, it is characterised in that described assistant crosslinking agent is
Cumyl peroxide or di-tert-butyl peroxide.
8. have the polyester fiber of energy-saving and temperature-regulating function as claimed in claim 1, it is characterised in that described Part I and
The mass ratio of Part II is 1/3 ~ 9/1.
9. the preparation method of the polyester fiber with energy-saving and temperature-regulating function any one of claim 1-8, its feature exists
In specific steps include：The first single screw extrusion machine and is respectively adopted in the raw material of the raw material of Part I and Part II
Two single screw extrusion machines are extruded, and carry out melt spinning using bicomponent fibre component or double structures point fiber sprinning assembly, are had
There is the polyester fiber of energy-saving and temperature-regulating function.
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| CN105968829B (en) * | 2016-05-27 | 2018-07-24 | 福建天利高新材料有限公司 | A kind of fretting map phase change paraffin material and preparation method thereof |
| CN107587207A (en) * | 2016-07-06 | 2018-01-16 | 中国石化仪征化纤有限责任公司 | One kind heating phase transformation core-skin fibre and preparation method thereof |
| CA3062277A1 (en) * | 2017-05-01 | 2018-11-08 | Dupont Polymers, Inc. | Composition and methods for coaxial devices including a phase change material |
| CN107513774A (en) * | 2017-08-24 | 2017-12-26 | 广东宝汇环保科技有限公司 | A kind of production method spun before PET bottle piece |
| CN107502977A (en) * | 2017-09-26 | 2017-12-22 | 界首市双鑫纺织有限公司 | A kind of preparation method of high-quality textile fabric |
| CN113846392B (en) * | 2021-11-16 | 2023-09-08 | 江苏江南高纤股份有限公司 | Sheath-core component synergistic thermal insulation and moisture absorption composite polyester fiber and preparation method thereof |
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| KR100696914B1 (en) * | 2000-10-19 | 2007-03-20 | 아웃래스트 테크날러지스 인코포레이티드 | Temperature adaptable textile fibers and method of preparing same |
| CN101845683B (en) * | 2010-05-07 | 2012-07-04 | 盈保纤维科技(仁化)有限公司 | Fibers capable of heat storage and temperature adjustment |
| CN101906670B (en) * | 2010-08-26 | 2011-12-14 | 东华大学 | Melt spinning solid-liquid composite phase change fiber spinning equipment and preparation method thereof |
| CN102505179B (en) * | 2011-10-13 | 2014-07-02 | 大连工业大学 | Preparation method for thermal-storage and temperature-regulated fibers |
| CN103881231B (en) * | 2014-03-25 | 2015-12-09 | 大连工业大学 | A kind of thermal storage and energy accumulation spacer bar based on ethylene-vinyl acetate copolymer and preparation method thereof |
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