CN106087080A - A kind of wet spinning technology being applicable to prepare Semen livistonae chinensis leaf fibre element regenerated fiber - Google Patents

A kind of wet spinning technology being applicable to prepare Semen livistonae chinensis leaf fibre element regenerated fiber Download PDF

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Publication number
CN106087080A
CN106087080A CN201610426067.0A CN201610426067A CN106087080A CN 106087080 A CN106087080 A CN 106087080A CN 201610426067 A CN201610426067 A CN 201610426067A CN 106087080 A CN106087080 A CN 106087080A
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China
Prior art keywords
chinensis leaf
fibre element
semen livistonae
livistonae chinensis
regenerated fiber
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Pending
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CN201610426067.0A
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Chinese (zh)
Inventor
贾永堂
聂伟利
于晖
黄钢
董凤春
曾显华
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Wuyi University
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Wuyi University
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Priority to CN201610426067.0A priority Critical patent/CN106087080A/en
Publication of CN106087080A publication Critical patent/CN106087080A/en
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/06Wet spinning methods
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D1/00Treatment of filament-forming or like material
    • D01D1/02Preparation of spinning solutions
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/12Stretch-spinning methods
    • D01D5/14Stretch-spinning methods with flowing liquid or gaseous stretching media, e.g. solution-blowing
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F2/00Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
    • D01F2/02Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from solutions of cellulose in acids, bases or salts

Abstract

The present invention relates to a kind of wet spinning technology being applicable to prepare Semen livistonae chinensis leaf fibre element regenerated fiber, described technique includes Semen livistonae chinensis leaf fibre element is dissolved in anhydrous Lithium chloride/dimethyl acetylamide mixed solvent the preparation preparing spinning liquid and the wet spinning technology carried out in following condition and range: dimethyl acetylamide volumetric concentration 0 30%, stretch bath temperature 30 DEG C 60 DEG C, draw ratio 1.2 1.8 times in spinning liquid temperature 35 DEG C~95 DEG C, coagulation bath temperature 15 DEG C~45 DEG C, coagulating bath;The Semen livistonae chinensis leaf fibre element regenerated fiber prepared by wet spinning technology in condition and range of the present invention has good mechanical property and regain, needs to become a kind of new tModified Cellulose Fibers.

Description

A kind of wet spinning technology being applicable to prepare Semen livistonae chinensis leaf fibre element regenerated fiber
Technical field
The present invention relates to that a kind of anhydrous Lithium chloride/dimethylacetamide solvent system dissolves after Semen livistonae chinensis leaf fibre element is wet Method spinning technique, belongs to plant regeneration fibre technology field, particularly one and is applicable to prepare Semen livistonae chinensis leaf fibre element regenerated fiber Wet spinning technology.
Background technology
In textile industry, tModified Cellulose Fibers is owing to source resource is abundant, environmental friendliness, goods take the spies such as comfortable Property is constantly subjected to the attention of people.Although its consumption proportion is not as synthetic fibers in recent years, but the most withered due to coal and oil Exhausting, serious " white pollution " that the non-degradable of synthetic fibers products waste causes in addition is day by day serious, is ploughed simultaneously The restriction of area, protofibre yield also receives certain restriction, and the demand of fiber is constantly increasing, although weaving Industry is changed to promoting added value direction by production scale expanding, but still needs to maintain a number of growth to meet state Inside and outside demand.In the coming years, the demand of fiber will have growth by a relatively large margin, and this makes renewable fibre resources Exploitation is particularly important, its be possible not only to increase fibre resources source, decrease simultaneously natural resources is taken and Dependence to non-renewable resources.People are made sight to have been turned to the regeneration with the characteristic such as renewable, green, degradable fine Dimension.
Semen livistonae chinensis leaf, as the raw material of tModified Cellulose Fibers, south China most area has distribution, especially in river Door is local more, and cultivation technique is fairly simple.Semen livistonae chinensis leaf aboundresources but the most not by comprehensive development and utilization, big portion Office is in the state run its course, and this also result in the waste of certain resource.Along with people are to healthy, the day of environmental protection based article Benefit is pursued, the effective development and utilization of Semen livistonae chinensis leaf, will bring certain economic and social benefit for locality.
Semen livistonae chinensis leaf fibre element regenerated fiber meets modern and produces and the demand of life, but in life, this based article is also Not finding, the document relevant to the technique of preparation Semen livistonae chinensis leaf fibre element regenerated fiber also has no report.The present invention is to continue from Pu Certain herbaceous plants with big flowers leaf extracts method (Publication No. CN105019288A) and the dissolving method (Publication No. of Semen livistonae chinensis cellulose of cellulose CN105017540A), after two inventions, the invention of the spinning technique of regenerated fiber is prepared by Semen livistonae chinensis leaf fibre element.Therefore, Semen livistonae chinensis leaf The regeneration spinning technique of cellulose is the key issue that the present invention needs to solve.
Summary of the invention
The technical problem to be solved is to provide a kind of being applicable to and prepares the wet of Semen livistonae chinensis leaf fibre element regenerated fiber Method spinning technique, the Semen livistonae chinensis leaf fibre element regenerated fiber that this technique prepares has good mechanical property and regain.
A kind of wet spinning technology being applicable to prepare Semen livistonae chinensis leaf fibre element regenerated fiber of the present invention, including following step Rapid:
The preparation of A Semen livistonae chinensis leaf fibre element spinning liquid: a is in the ratio of anhydrous Lithium chloride solid 80 grams per liter, by anhydrous Lithium chloride solid It is dissolved in dimethylacetamide solvent, makes anhydrous Lithium chloride/dimethyl acetylamide mixed solvent;B presses Semen livistonae chinensis leaf fibre element 60 The ratio of grams per liter, is dissolved in Semen livistonae chinensis leaf fibre element in anhydrous Lithium chloride/dimethyl acetylamide mixed solvent, prepares spinning liquid;
B wet spinning: in the wet-spinning frame fluid reservoir that the spinning liquid prepared in step A is poured into, heating wet-spinning frame storage Flow container, after in fluid reservoir, spinning liquid temperature reaches balance and stability: 1. spinning liquid passes through dosing pump, filter, sprays from spinneret cap Go out;2. the coagulating bath coagulation forming being directly over being made up of dimethyl acetylamide and water by the spinning liquid sprayed by spinneret cap is formed As-spun fibre;3. the as-spun fibre of molding in coagulating bath is introduced stretch bath by deflector roll;4. as-spun fibre enters and is made up of water Stretch bath in, control the draw ratio of fiber by changing stretch bath two ends deflector roll speed, thus as-spun fibre carried out Stretching;5. the as-spun fibre after stretching is wound by take-up roll;5. coiled fiber is dried, prepare Semen livistonae chinensis leaf fibre element Regenerated fiber.
A kind of wet spinning technology being applicable to prepare Semen livistonae chinensis leaf fibre element regenerated fiber, in described step B in fluid reservoir Spinning liquid temperature be set to 35 DEG C~95 DEG C.
A kind of wet spinning technology being applicable to prepare Semen livistonae chinensis leaf fibre element regenerated fiber, in described step B in coagulating bath The volumetric concentration of dimethyl acetylamide is set to 0~30%.
A kind of wet spinning technology being applicable to prepare Semen livistonae chinensis leaf fibre element regenerated fiber, solidifies bath temperature in described step B Degree is set to 15 DEG C~60 DEG C.
A kind of wet spinning technology being applicable to prepare Semen livistonae chinensis leaf fibre element regenerated fiber, stretches bath temperature in described step B Degree is set to 30 DEG C~70 DEG C.
A kind of wet spinning technology being applicable to prepare Semen livistonae chinensis leaf fibre element regenerated fiber, draw ratio in described step B It is set to 1.2~1.8.
The present invention is that the Semen livistonae chinensis leaf fibre element utilizing dissolving to prepare is molten after the extraction and dissolving of Semen livistonae chinensis leaf fibre element Liquid, prepares Semen livistonae chinensis leaf fibre element regenerated fiber by wet spinning technology, and the fiber obtained has good mechanical property and returns Tide rate, is expected to become a kind of new tModified Cellulose Fibers.
Accompanying drawing explanation
Fig. 1 wet spinning technology flow chart.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is expanded on further.
Embodiment 1
The preparation of A Semen livistonae chinensis leaf fibre element spinning liquid: a is in the ratio of anhydrous Lithium chloride solid 80 grams per liter, by 800 grams of anhydrous chlorinations Lithium solid is dissolved in dimethylacetamide solvent, makes anhydrous Lithium chloride/dimethyl acetylamide mixed solvent 10 liters;By Semen livistonae chinensis leaf 600 grams of Semen livistonae chinensis leaf fibre elements are dissolved in 10 liters of mixed solvents that a step prepares, prepare spinning by the ratio of cellulose 60 grams per liter Liquid 10 liters;
B wet spinning: in the wet-spinning frame fluid reservoir pour into the 10 liters of spinning liquid prepared in step A, heat wet spinning Machine fluid reservoir is to 65 DEG C, after in fluid reservoir, spinning liquid temperature reaches balance and stability: 1. spinning liquid passes through dosing pump, filter, Spray from spinneret cap;2. the spinning liquid sprayed by spinneret cap is added directly into temperature be 30 DEG C, dimethyl acetylamide concentration be 30%, in the coagulating bath that is made up of dimethyl acetylamide and water, coagulation forming forms as-spun fibre;3. by molding in coagulating bath As-spun fibre introduces, by deflector roll, the stretch bath that temperature is 40 DEG C;4., during as-spun fibre enters the stretch bath being made up of water, pass through It is 1.2 times that change stretch bath two ends deflector roll speed controls the draw ratio of fiber, stretches as-spun fibre;5. will stretching After as-spun fibre be wound by take-up roll;5. coiled fiber is dried, prepare Semen livistonae chinensis leaf fibre element regenerated fiber.
By said method of the present invention, the average fracture strength of the Semen livistonae chinensis leaf fibre element regenerated fiber of preparation reaches 1.351 cN/dtex。
Embodiment 2
The preparation of A Semen livistonae chinensis leaf fibre element spinning liquid: a is in the ratio of anhydrous Lithium chloride solid 80 grams per liter, by 800 grams of anhydrous chlorinations Lithium solid is dissolved in dimethylacetamide solvent, makes anhydrous Lithium chloride/dimethyl acetylamide mixed solvent 10 liters;By Semen livistonae chinensis leaf 600 grams of Semen livistonae chinensis leaf fibre elements are dissolved in 10 liters of mixed solvents that a step prepares, prepare spinning by the ratio of cellulose 60 grams per liter Liquid 10 liters;
B wet spinning: in the wet-spinning frame fluid reservoir pour into the 10 liters of spinning liquid prepared in step A, heat wet spinning Machine fluid reservoir is to 95 DEG C, after in fluid reservoir, spinning liquid temperature reaches balance and stability: 1. spinning liquid passes through dosing pump, filter, Spray from spinneret cap;2. the spinning liquid sprayed by spinneret cap is added directly into temperature be 30 DEG C, dimethyl acetylamide concentration be 10%, in the coagulating bath that is made up of dimethyl acetylamide and water, coagulation forming forms as-spun fibre;3. by molding in coagulating bath As-spun fibre introduces, by deflector roll, the stretch bath that temperature is 30 DEG C;4., during as-spun fibre enters the stretch bath being made up of water, pass through It is 1.5 times that change stretch bath two ends deflector roll speed controls the draw ratio of fiber, stretches as-spun fibre;5. will stretching After as-spun fibre be wound by take-up roll;5. coiled fiber is dried, prepare Semen livistonae chinensis leaf fibre element regenerated fiber.
By said method of the present invention, the average fracture strength of the Semen livistonae chinensis leaf fibre element regenerated fiber of preparation reaches 1.630 cN/dtex.Regain reaches
Embodiment 3
The preparation of A Semen livistonae chinensis leaf fibre element spinning liquid: a is in the ratio of anhydrous Lithium chloride solid 80 grams per liter, by 800 grams of anhydrous chlorinations Lithium solid is dissolved in dimethylacetamide solvent, makes anhydrous Lithium chloride/dimethyl acetylamide mixed solvent 10 liters;By Semen livistonae chinensis leaf 600 grams of Semen livistonae chinensis leaf fibre elements are dissolved in 10 liters of mixed solvents that a step prepares, prepare spinning by the ratio of cellulose 60 grams per liter Liquid 10 liters;
B wet spinning: in the wet-spinning frame fluid reservoir pour into the 10 liters of spinning liquid prepared in step A, heat wet spinning Machine fluid reservoir is to 35 DEG C, after in fluid reservoir, spinning liquid temperature reaches balance and stability: 1. spinning liquid passes through dosing pump, filter, Spray from spinneret cap;2. the spinning liquid sprayed by spinneret cap is added directly into temperature be 45 DEG C, dimethyl acetylamide concentration be 10%, in the coagulating bath that is made up of dimethyl acetylamide and water, coagulation forming forms as-spun fibre;3. by molding in coagulating bath As-spun fibre introduces, by deflector roll, the stretch bath that temperature is 40 DEG C;4., during as-spun fibre enters the stretch bath being made up of water, pass through It is 1.5 times that change stretch bath two ends deflector roll speed controls the draw ratio of fiber, stretches as-spun fibre;5. will stretching After as-spun fibre be wound by take-up roll;5. coiled fiber is dried, prepare Semen livistonae chinensis leaf fibre element regenerated fiber.
By said method of the present invention, the average fracture strength of the Semen livistonae chinensis leaf fibre element regenerated fiber of preparation reaches 1.609 cN/dtex。
Embodiment 4
The preparation of A Semen livistonae chinensis leaf fibre element spinning liquid: a is in the ratio of anhydrous Lithium chloride solid 80 grams per liter, by 800 grams of anhydrous chlorinations Lithium solid is dissolved in dimethylacetamide solvent, makes anhydrous Lithium chloride/dimethyl acetylamide mixed solvent 10 liters;By Semen livistonae chinensis leaf 600 grams of Semen livistonae chinensis leaf fibre elements are dissolved in 10 liters of mixed solvents that a step prepares, prepare spinning by the ratio of cellulose 60 grams per liter Liquid 10 liters;
B wet spinning: in the wet-spinning frame fluid reservoir pour into the 10 liters of spinning liquid prepared in step A, heat wet spinning Machine fluid reservoir is to 65 DEG C, after in fluid reservoir, spinning liquid temperature reaches balance and stability: 1. spinning liquid passes through dosing pump, filter, Spray from spinneret cap;2. the spinning liquid sprayed by spinneret cap is added directly into temperature be 15 DEG C, dimethyl acetylamide concentration be 10%, in the coagulating bath that is made up of dimethyl acetylamide and water, coagulation forming forms as-spun fibre;3. by molding in coagulating bath As-spun fibre introduces, by deflector roll, the stretch bath that temperature is 60 DEG C;4., during as-spun fibre enters the stretch bath being made up of water, pass through It is 1.5 times that change stretch bath two ends deflector roll speed controls the draw ratio of fiber, stretches as-spun fibre;5. will stretching After as-spun fibre be wound by take-up roll;5. coiled fiber is dried, prepare Semen livistonae chinensis leaf fibre element regenerated fiber.
By said method of the present invention, the average fracture strength of the Semen livistonae chinensis leaf fibre element regenerated fiber of preparation reaches 1.743 cN/dtex。
Embodiment 5
The preparation of A Semen livistonae chinensis leaf fibre element spinning liquid: a is in the ratio of anhydrous Lithium chloride solid 80 grams per liter, by 800 grams of anhydrous chlorinations Lithium solid is dissolved in dimethylacetamide solvent, makes anhydrous Lithium chloride/dimethyl acetylamide mixed solvent 10 liters;By Semen livistonae chinensis leaf 600 grams of Semen livistonae chinensis leaf fibre elements are dissolved in 10 liters of mixed solvents that a step prepares, prepare spinning by the ratio of cellulose 60 grams per liter Liquid 10 liters;
B wet spinning: in the wet-spinning frame fluid reservoir pour into the 10 liters of spinning liquid prepared in step A, heat wet spinning Machine fluid reservoir is to 65 DEG C, after in fluid reservoir, spinning liquid temperature reaches balance and stability: 1. spinning liquid passes through dosing pump, filter, Spray from spinneret cap;2. the spinning liquid sprayed by spinneret cap is added directly into temperature be 30 DEG C, dimethyl acetylamide concentration be 0%, in the coagulating bath that is made up of dimethyl acetylamide and water, coagulation forming forms as-spun fibre;3. by molding in coagulating bath As-spun fibre introduces, by deflector roll, the stretch bath that temperature is 40 DEG C;4., during as-spun fibre enters the stretch bath being made up of water, pass through It is 1.8 times that change stretch bath two ends deflector roll speed controls the draw ratio of fiber, stretches as-spun fibre;5. will stretching After as-spun fibre be wound by take-up roll;5. coiled fiber is dried, prepare Semen livistonae chinensis leaf fibre element regenerated fiber.
By said method of the present invention, the average fracture strength of the Semen livistonae chinensis leaf fibre element regenerated fiber of preparation reaches 1.985 CN/dtex, regain reaches 14.51%.
It addition, five specific embodiments of the present invention are to be entered the present invention by embodiment in scope The explanation of one step, and not limitation of the invention further, make the corresponding of other forms according to the foregoing of the present invention Change, equivalent belong to protection scope of the present invention.

Claims (6)

1. a kind of wet spinning technology being applicable to prepare Semen livistonae chinensis leaf fibre element regenerated fiber of the present invention, it is characterised in that include The following step:
The preparation of A Semen livistonae chinensis leaf fibre element spinning liquid: a is in the ratio of anhydrous Lithium chloride solid 80 grams per liter, and anhydrous Lithium chloride is solid Body is dissolved in dimethylacetamide solvent, makes anhydrous Lithium chloride/dimethyl acetylamide mixed solvent;B is by Semen livistonae chinensis leaf fibre element The ratio of 60 grams per liters, is dissolved in Semen livistonae chinensis leaf fibre element in anhydrous Lithium chloride/dimethyl acetylamide mixed solvent, prepares spinning liquid;
B wet spinning: in the wet-spinning frame fluid reservoir that the spinning liquid prepared in step A is poured into, heating wet-spinning frame storage Flow container, after in fluid reservoir, spinning liquid temperature reaches balance and stability: 1. spinning liquid passes through dosing pump, filter, sprays from spinneret cap Go out;2. the coagulating bath coagulation forming being directly over being made up of dimethyl acetylamide and water by the spinning liquid sprayed by spinneret cap is formed As-spun fibre;3. the as-spun fibre of molding in coagulating bath is introduced stretch bath by deflector roll;4. as-spun fibre enters and is made up of water Stretch bath in, control the draw ratio of fiber by changing stretch bath two ends deflector roll speed, thus as-spun fibre carried out Stretching;5. the as-spun fibre after stretching is wound by take-up roll;5. coiled fiber is dried, prepare Semen livistonae chinensis leaf fibre element Regenerated fiber.
2. according to a kind of wet spinning technology being applicable to prepare Semen livistonae chinensis leaf fibre element regenerated fiber described in right 1, its feature The spinning liquid temperature being in described step B in fluid reservoir is set to 35 DEG C~95 DEG C.
3. according to a kind of wet spinning technology being applicable to prepare Semen livistonae chinensis leaf fibre element regenerated fiber described in right 1, its feature It is in described step B that in coagulating bath, the volumetric concentration of dimethyl acetylamide is set to 0~30%.
4. according to a kind of wet spinning technology being applicable to prepare Semen livistonae chinensis leaf fibre element regenerated fiber described in right 1, its feature It is in described step B that coagulation bath temperature is set to 15 DEG C~60 DEG C.
5. according to a kind of wet spinning technology being applicable to prepare Semen livistonae chinensis leaf fibre element regenerated fiber described in right 1, its feature It is in described step B that stretch bath temperature is set to 30 DEG C~70 DEG C.
6. according to a kind of wet spinning technology being applicable to prepare Semen livistonae chinensis leaf fibre element regenerated fiber described in right 1, its feature It is in described step B that draw ratio is set to 1.2~1.8.
CN201610426067.0A 2016-06-16 2016-06-16 A kind of wet spinning technology being applicable to prepare Semen livistonae chinensis leaf fibre element regenerated fiber Pending CN106087080A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106929929A (en) * 2017-03-21 2017-07-07 昆明理工大学 A kind of preparation method of the cellulose spin dope for electrostatic spinning
CN110872732A (en) * 2018-08-30 2020-03-10 奥若泰克股份有限公司 Method and device for spinning filaments by deflection
CN113897709A (en) * 2021-10-29 2022-01-07 上海纳米技术及应用国家工程研究中心有限公司 Regenerated cellulose wet spinning
CN115613157A (en) * 2022-10-26 2023-01-17 西安工程大学 Preparation method of high-strength color artificial cotton based on waste cotton textiles

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106929929A (en) * 2017-03-21 2017-07-07 昆明理工大学 A kind of preparation method of the cellulose spin dope for electrostatic spinning
CN106929929B (en) * 2017-03-21 2019-06-07 昆明理工大学 A kind of preparation method of the cellulose spin dope for electrostatic spinning
CN110872732A (en) * 2018-08-30 2020-03-10 奥若泰克股份有限公司 Method and device for spinning filaments by deflection
CN110872732B (en) * 2018-08-30 2022-02-15 奥若泰克股份有限公司 Method and device for spinning filaments by deflection
CN113897709A (en) * 2021-10-29 2022-01-07 上海纳米技术及应用国家工程研究中心有限公司 Regenerated cellulose wet spinning
CN115613157A (en) * 2022-10-26 2023-01-17 西安工程大学 Preparation method of high-strength color artificial cotton based on waste cotton textiles
CN115613157B (en) * 2022-10-26 2024-01-02 西安工程大学 Preparation method of high-strength colored artificial cotton based on waste cotton textiles

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