CN109078620A - A method of adsorbent for heavy metal is prepared with graft modification cotton fiber - Google Patents
A method of adsorbent for heavy metal is prepared with graft modification cotton fiber Download PDFInfo
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- CN109078620A CN109078620A CN201811017265.7A CN201811017265A CN109078620A CN 109078620 A CN109078620 A CN 109078620A CN 201811017265 A CN201811017265 A CN 201811017265A CN 109078620 A CN109078620 A CN 109078620A
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/264—Synthetic macromolecular compounds derived from different types of monomers, e.g. linear or branched copolymers, block copolymers, graft copolymers
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
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- D06M11/07—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
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- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/38—Oxides or hydroxides of elements of Groups 1 or 11 of the Periodic System
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- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
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- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/144—Alcohols; Metal alcoholates
- D06M13/148—Polyalcohols, e.g. glycerol or glucose
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- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
- D06M13/325—Amines
- D06M13/332—Di- or polyamines
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
- B01J2220/4825—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
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- D06M2101/02—Natural fibres, other than mineral fibres
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Abstract
The invention discloses a kind of methods for preparing adsorbent for heavy metal with graft modification cotton fiber, and oxidized cotton fiber is placed in tetraethylenepentamine solution, heat graft reaction, are sufficiently freeze-dried after washing, must be grafted the modified cotton fiber of tetraethylenepentamine;NaOH aqueous solution, dehydrated alcohol, epoxychloropropane are sequentially added into oxidized cotton fiber, after heating graft reaction in a water bath, are washed to neutrality, with acetone washing, are dried to obtain epoxy cotton fiber;Deionized water, Na are sequentially added into gained epoxy cotton fiber2CO3, diethylenetriamine, graft reaction under the conditions of nitrogen protection is washed to neutrality, dries to obtain ion-exchange fibre;It is uniformly mixed with the modified cotton fiber of gained grafting tetraethylenepentamine, adsorbent for heavy metal is made.
Description
Technical field
The invention belongs to cotton fiber application fields, and in particular to a kind of graft modification cotton fiber preparation heavy metal ion suction
Attached dose of method.
Background technique
Heavy metal pollution refers to the environmental pollution as caused by heavy metal or its compound, enters people by food and water
Strong interaction occurs for meeting and protein and various enzymes after body, them is made to lose activity;It may also be in certain devices of human body
It is enriched in official, causes human body acute poisoning, subacute poisoning or slow poisoning etc., very big harm is generated to human body.Therefore it controls
Reason heavy metal pollution problem is increasingly subject to the attention of people.
Heavy metal pollution of water body has become global environmental problem.Heavy metal in environment cannot be degraded, big portion
Point heavy metal exists in the form of an ion in water body, colorless and odorless, into food chain after long-term accumulation, enable organism toxicosis, after
Fruit is serious, has great threat to environmental and human health impacts.In face of increasingly serious heavy metal pollution of water body, effectively go to remove water
In body while heavy metal, realize the material and method of the easy detection and concentration early warning of Heavy Metals in Waters, be there is an urgent need to
's.
Summary of the invention
The purpose of the present invention is being directed to existing problem, a kind of graft modification cotton fiber preparation heavy metal ion is provided
The method of adsorbent can adsorb contents of many kinds of heavy metal ion according to the adsorbent that this method makes, solve the problems, such as water pollution.
The present invention is achieved by the following technical solutions:
A method of adsorbent for heavy metal is prepared with graft modification cotton fiber, which comprises the steps of:
(1) preparation of oxidized cotton fiber:
10-20 parts of cotton fibers are impregnated into 1-2h, mistake in the sodium hydroxide solution that 94-96 DEG C of concentration is 20g/L by bath raio 1:50
After filter washing, drying, 1-2h is impregnated in the sodium hydroxide solution that mass fraction is 18% by bath raio 1:30, washing to neutrality is taken out
After filter, drying, it is placed in sodium periodate solution by bath raio 1:30, oxidation reaction 2-3h, it is molten to place into glycerine at 70-73 DEG C
After impregnating 20-25h in liquid, washing and drying obtains oxidized cotton fiber, is divided into two parts, for use;
(2) oxidized cotton fiber is grafted tetraethylenepentamine:
Gained oxidized cotton fiber in a (1) is placed in tetraethylenepentamine solution by bath raio 1:50, is grafted at 70-73 DEG C anti-
1-2h is answered, is sufficiently freeze-dried after washing, the modified cotton fiber of tetraethylenepentamine must be grafted;
(3) preparation of epoxy cotton fiber:
To sequentially added in gained oxidized cotton fiber in another (1) 250-500 parts of NaOH aqueous solutions, 13-26 parts of dehydrated alcohols,
58-116 parts of epoxychloropropane are washed to neutrality, with acetone washing 3-5 after heating graft reaction 6-8h in 70-73 DEG C of water-bath
It is secondary, dry to obtain epoxy cotton fiber;
(4) preparation of adsorbent for heavy metal:
143-286 parts of deionized waters, 2-4 parts of Na are sequentially added into (3) middle gained epoxy cotton fiber2CO3, 11-22 parts of diethyls
Alkene triamine in 54-56 DEG C of graft reaction 2-3h, is washed to neutrality, dries to obtain ion-exchange fibre under the conditions of nitrogen protection;
It is uniformly mixed with resulting material in (2), adsorbent for heavy metal is made.
Further, the concentration of step (1) meso-periodic acid sodium solution is 20g/L, and the concentration of glycerin solution is 0.1mol/
L。
Further, the concentration of tetraethylenepentamine solution is 20g/L in step (2).
Further, NaOH concentration of aqueous solution is 8% in step (3).
The present invention has the advantage that compared with prior art
(1) using cotton fiber as carrier, cotton fiber is activated using certain density NaOH solution, it is activated after cotton it is fine
Dimension crystallinity and crystallite dimension all reduce;Tetraethylenepentamine, which is grafted, by the cotton fiber after aoxidizing to dialdehyde is successfully prepared modification
Cotton fiber adsorbent for heavy metal;The longitudinal stripe that the preprocessed oxidation rear surface of cotton fiber occurs disappears after modification;Cotton
Contain a large amount of amino and hydroxyl isoreactivity site on fiber, absorption can be reached by being coordinated chelation with heavy metal ion
The purpose of removing heavy metals;Adsorbent belongs to mono layer adsorption, adsorbent to the adsorption process of heavy metal ion, this adsorption process
The distribution of adsorption site is relatively uniform.
(2) using oxidized cotton fiber as raw material, using epoxychloropropane and diethylenetriamine as grafted monomers, pass through graft modification
It is prepared for the ion exchange material with adsorption function;Surface by smooth becomes coarse to cotton fiber after processing, and surface has largely
Graininess or villiform substance invest above;Corresponding active group is introduced on cotton fiber molecular structure;Illustrate graft modification
The molecular structure and mode of appearance of cotton fiber are changed, epoxychloropropane and diethylenetriamine are successfully grafted on cotton fiber.
Specific embodiment
Embodiment 1
A method of adsorbent for heavy metal is prepared with graft modification cotton fiber, which comprises the steps of:
(1) preparation of oxidized cotton fiber:
10 parts of cotton fibers are impregnated into 1h by bath raio 1:50 in the sodium hydroxide solution that 94-96 DEG C of concentration is 20g/L, cross diafiltration
After washing, drying, 1h is impregnated in the sodium hydroxide solution that mass fraction is 18% by bath raio 1:30, washing to neutrality is filtered, dried
After dry, it is placed in sodium periodate solution by bath raio 1:30, oxidation reaction 2h, places into glycerin solution and soak at 70-73 DEG C
After stain 20h, washing and drying obtains oxidized cotton fiber, is divided into two parts, for use;
(2) oxidized cotton fiber is grafted tetraethylenepentamine:
Gained oxidized cotton fiber in a (1) is placed in tetraethylenepentamine solution by bath raio 1:50, is grafted at 70-73 DEG C anti-
1h is answered, is sufficiently freeze-dried after washing, the modified cotton fiber of tetraethylenepentamine must be grafted;
(3) preparation of epoxy cotton fiber:
250 parts of NaOH aqueous solutions, 13 parts of dehydrated alcohols, 58 parts of rings are sequentially added into another (1) middle gained oxidized cotton fiber
Oxygen chloropropane is washed to neutrality, with acetone washing 3 times, dries to obtain epoxy after heating graft reaction 6h in 70-73 DEG C of water-bath
Cotton fiber;
(4) preparation of adsorbent for heavy metal:
143 parts of deionized waters, 2 parts of Na are sequentially added into (3) middle gained epoxy cotton fiber2CO3, 11 parts of diethylenetriamines,
Under the conditions of nitrogen protection, in 54-56 DEG C of graft reaction 2h, it is washed to neutrality, dries to obtain ion-exchange fibre;By its in (2)
Resulting material is uniformly mixed, and adsorbent for heavy metal is made.
Further, the concentration of step (1) meso-periodic acid sodium solution is 20g/L, and the concentration of glycerin solution is 0.1mol/
L。
Further, the concentration of tetraethylenepentamine solution is 20g/L in step (2).
Further, NaOH concentration of aqueous solution is 8% in step (3).
Embodiment 2
A method of adsorbent for heavy metal is prepared with graft modification cotton fiber, which comprises the steps of:
(1) preparation of oxidized cotton fiber:
20 parts of cotton fibers are impregnated into 2h by bath raio 1:50 in the sodium hydroxide solution that 94-96 DEG C of concentration is 20g/L, cross diafiltration
After washing, drying, 2h is impregnated in the sodium hydroxide solution that mass fraction is 18% by bath raio 1:30, washing to neutrality is filtered, dried
After dry, it is placed in sodium periodate solution by bath raio 1:30, oxidation reaction 3h, places into glycerin solution and soak at 70-73 DEG C
After stain 25h, washing and drying obtains oxidized cotton fiber, is divided into two parts, for use;
(2) oxidized cotton fiber is grafted tetraethylenepentamine:
Gained oxidized cotton fiber in a (1) is placed in tetraethylenepentamine solution by bath raio 1:50, is grafted at 70-73 DEG C anti-
2h is answered, is sufficiently freeze-dried after washing, the modified cotton fiber of tetraethylenepentamine must be grafted;
(3) preparation of epoxy cotton fiber:
500 parts of NaOH aqueous solutions, 26 parts of dehydrated alcohols, 116 parts of rings are sequentially added into another (1) middle gained oxidized cotton fiber
Oxygen chloropropane is washed to neutrality, with acetone washing 5 times, dries to obtain epoxy after heating graft reaction 8h in 70-73 DEG C of water-bath
Cotton fiber;
(4) preparation of adsorbent for heavy metal:
286 parts of deionized waters, 4 parts of Na are sequentially added into (3) middle gained epoxy cotton fiber2CO3, 22 parts of diethylenetriamines,
Under the conditions of nitrogen protection, in 54-56 DEG C of graft reaction 3h, it is washed to neutrality, dries to obtain ion-exchange fibre;By its in (2)
Resulting material is uniformly mixed, and adsorbent for heavy metal is made.
Further, the concentration of step (1) meso-periodic acid sodium solution is 20g/L, and the concentration of glycerin solution is 0.1mol/
L。
Further, the concentration of tetraethylenepentamine solution is 20g/L in step (2).
Further, NaOH concentration of aqueous solution is 8% in step (3).
There is excellent degradability according to the polybag of the method for the present invention production, soil is carried out to polybag and buries degradation in fact
It tests, discovery polybag degradability in the basic soil of high fertility is excellent;Degradable plastic bag can be in 9 weeks degradation times
It is almost biodegradable, degradability is superior;
Contents of many kinds of heavy metal ion can be adsorbed according to the adsorbent that the present embodiment makes, solves the problems, such as water pollution;It is in pH
Under the conditions of 3-4, temperature are 35 DEG C, adsorption time is 60min, Pb2+、Cd2+、Cu2+、Ni2+Initial concentration be 500mg/L, change
Property cotton fiber adsorbent is to Pb2+、Cd2+、Cu2+、Ni2+Maximum adsorption capacity be respectively as follows: 722mg/g, 504mg/g, 335mg/g,
379mg/g。
Claims (4)
1. a kind of method for preparing adsorbent for heavy metal with graft modification cotton fiber, which comprises the steps of:
(1) preparation of oxidized cotton fiber:
10-20 parts of cotton fibers are impregnated into 1-2h, mistake in the sodium hydroxide solution that 94-96 DEG C of concentration is 20g/L by bath raio 1:50
After filter washing, drying, 1-2h is impregnated in the sodium hydroxide solution that mass fraction is 18% by bath raio 1:30, washing to neutrality is taken out
After filter, drying, it is placed in sodium periodate solution by bath raio 1:30, oxidation reaction 2-3h, it is molten to place into glycerine at 70-73 DEG C
After impregnating 20-25h in liquid, washing and drying obtains oxidized cotton fiber, is divided into two parts, for use;
(2) oxidized cotton fiber is grafted tetraethylenepentamine:
Gained oxidized cotton fiber in a (1) is placed in tetraethylenepentamine solution by bath raio 1:50, is grafted at 70-73 DEG C anti-
1-2h is answered, is sufficiently freeze-dried after washing, the modified cotton fiber of tetraethylenepentamine must be grafted;
(3) preparation of epoxy cotton fiber:
To sequentially added in gained oxidized cotton fiber in another (1) 250-500 parts of NaOH aqueous solutions, 13-26 parts of dehydrated alcohols,
58-116 parts of epoxychloropropane are washed to neutrality, with acetone washing 3-5 after heating graft reaction 6-8h in 70-73 DEG C of water-bath
It is secondary, dry to obtain epoxy cotton fiber;
(4) preparation of adsorbent for heavy metal:
143-286 parts of deionized waters, 2-4 parts of Na are sequentially added into (3) middle gained epoxy cotton fiber2CO3, 11-22 parts of divinyls
Triamine in 54-56 DEG C of graft reaction 2-3h, is washed to neutrality, dries to obtain ion-exchange fibre under the conditions of nitrogen protection;It will
It is uniformly mixed with resulting material in (2), and adsorbent for heavy metal is made.
2. a kind of method for preparing adsorbent for heavy metal with graft modification cotton fiber according to claim 1, special
Sign is that the concentration of step (1) meso-periodic acid sodium solution is 20g/L, and the concentration of glycerin solution is 0.1mol/L.
3. a kind of method for preparing adsorbent for heavy metal with graft modification cotton fiber according to claim 1, special
Sign is that the concentration of tetraethylenepentamine solution is 20g/L in step (2).
4. a kind of method for preparing adsorbent for heavy metal with graft modification cotton fiber according to claim 1, special
Sign is that NaOH concentration of aqueous solution is 8% in step (3).
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Cited By (4)
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CN110142030A (en) * | 2019-04-02 | 2019-08-20 | 广东宏庭环保科技有限公司 | A kind of preparation method of the efficient formaldehyde adsorbent material based on active carbon |
CN111408354A (en) * | 2020-03-30 | 2020-07-14 | 杭州师范大学钱江学院 | Solid phase extracting agent based on bio-fiber mask leftover material and preparation method thereof |
CN112806646A (en) * | 2021-03-23 | 2021-05-18 | 上海喂闹信息科技有限公司 | Preparation method of mask with long-acting sterilization function |
CN115538149A (en) * | 2022-09-28 | 2022-12-30 | 安徽深呼吸纺织科技有限公司 | Antibacterial skin-friendly textile material and preparation method thereof |
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CN104815617A (en) * | 2015-04-27 | 2015-08-05 | 宁夏医科大学 | Preparing method of ephedra amination waste biosorbent |
CN105013447A (en) * | 2015-07-01 | 2015-11-04 | 南通大学 | Preparation method of modified cellulose heavy metal adsorbent |
RU2640547C1 (en) * | 2016-12-19 | 2018-01-09 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Ивановский государственный химико-технологический университет" (ИГХТУ) | Method for modifying sorbents based on cellulose for extracting ions of heavy metals from water solutions |
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CN104815617A (en) * | 2015-04-27 | 2015-08-05 | 宁夏医科大学 | Preparing method of ephedra amination waste biosorbent |
CN105013447A (en) * | 2015-07-01 | 2015-11-04 | 南通大学 | Preparation method of modified cellulose heavy metal adsorbent |
RU2640547C1 (en) * | 2016-12-19 | 2018-01-09 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Ивановский государственный химико-технологический университет" (ИГХТУ) | Method for modifying sorbents based on cellulose for extracting ions of heavy metals from water solutions |
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
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CN110142030A (en) * | 2019-04-02 | 2019-08-20 | 广东宏庭环保科技有限公司 | A kind of preparation method of the efficient formaldehyde adsorbent material based on active carbon |
CN110142030B (en) * | 2019-04-02 | 2021-10-29 | 山西龙清环保新材料有限公司 | Preparation method of efficient formaldehyde adsorption material based on activated carbon |
CN111408354A (en) * | 2020-03-30 | 2020-07-14 | 杭州师范大学钱江学院 | Solid phase extracting agent based on bio-fiber mask leftover material and preparation method thereof |
CN111408354B (en) * | 2020-03-30 | 2022-11-25 | 杭州师范大学钱江学院 | Solid phase extracting agent based on bio-fiber mask leftover material and preparation method thereof |
CN112806646A (en) * | 2021-03-23 | 2021-05-18 | 上海喂闹信息科技有限公司 | Preparation method of mask with long-acting sterilization function |
CN115538149A (en) * | 2022-09-28 | 2022-12-30 | 安徽深呼吸纺织科技有限公司 | Antibacterial skin-friendly textile material and preparation method thereof |
CN115538149B (en) * | 2022-09-28 | 2023-11-17 | 安徽深呼吸纺织科技有限公司 | Antibacterial skin-friendly textile material and preparation method thereof |
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Application publication date: 20181225 |