CN102744996B - Graphene oxide inkjet recording material and manufacturing method thereof - Google Patents
Graphene oxide inkjet recording material and manufacturing method thereof Download PDFInfo
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Abstract
The invention relates to a graphene oxide inkjet recording material and a manufacturing method of the graphene oxide inkjet recording material, which aim at solving the technical problems that the existing expansion type ink absorption layer inkjet recording material slowly absorbs ink and the interspace type ink absorption layer inkjet recording material likely has folded flaws. The graphene oxide inkjet recording material provided by the invention is composed of a base and a graphene oxide/acrylic copolymer coated on the base. The manufacturing method provided by the invention comprises the following steps: 1, oxidating graphite; 2, purifying the graphene oxide; 3, functionalizing the graphene oxide; 4, adding double-bond graphite oxide, acrylic acid, water and initiator in a reactor to react under the protection of insert gas so as to obtain the graphene oxide/acrylic copolymer, and then coating the graphene oxide/acrylic copolymer on the base to obtain the graphene oxide inkjet recording material. The graphene oxide inkjet recording material provided by the invention can be applied to the field of inkjet printing.
Description
Technical field
The present invention relates to graphene composite material and preparation method thereof.
Background technology
Along with the progress of modern science and technology, digital technology is developed rapidly in the world today.The thing followed is PC, network, day by day popularizing of digital camera and developing rapidly of electronic publishing system, and various digitized video hard copies output is more and more important.Due to ink-jet printer low price, print quality is high, has become gradually the main selection of office and family.Inkjet technology is made up of three parts: ink-jet printer, marking ink and inkjet printing recording medium.In the production process of ink jet recording medium, ink absorbing layer technology is its core technology, is directly determining the quality of finished product, also indicates the technological progress of ink jet recording medium product.The operation principle of ink mist recording is: it is to spray micron-sized nozzle from aperture that liquid ink heating or pressurization are made to ink, and the ink particle splashing is selectively attached to according to given signal and on the surface of accepting material, forms image or word.In general, ink mist recording process is made up of double teacher: ink particle is ejected into the surface of stock → permeate with stock Surface Contact → quilt → absorb → form a little fast.That is: 1. 2. contact collides and 3. forms point 4. infiltration is 5. dry.Ink jet layer can be divided into two types: the ink absorbing layer that, mainly comprises water-soluble polymer; Two, mainly comprise the ink absorbing layer of inorganic pigment and resin binder; The blotting principle of the first type is mainly to utilize the expansion absorption ink of water-soluble resin, and therefore it is also referred to as intumescent ink absorbing layer.In the ink absorbing layer of this type, because it forms continuous uniform films, glossiness is good, but blotting speed is slow, causes printing rear rate of drying low; The second mainly utilizes the space between pigment to absorb ink, and therefore it is also known as air gap type ink absorbing layer.The ink absorbing layer of this type has fabulous ink absorption, but glossiness is inferior, and recording materials are when folding, can produce fold cracks.
Summary of the invention
The present invention will solve that the blotting speed of existing intumescent ink absorbing layer ink jet recording materials is slow, the technical problem of the easy generation fold cracks of air gap type ink absorbing layer ink jet recording materials, and a kind of graphene oxide ink jet recording materials and preparation method thereof is provided.
A kind of graphene oxide ink jet recording materials of the present invention is by substrate and is coated in suprabasil graphene oxide/acrylic copolymer and forms, graphene oxide/acrylic copolymer is wherein by pressing two key graphene oxides, acrylic acid, water and initiator for reaction are made, wherein two key graphene oxides and acrylic acid mass ratio 1: (10～100), the quality of water is 10～50 times of acrylic acid quality, the quality of initator is 0.1～2% of acrylic acid quality, two key graphene oxides are (1～5) by graphene oxide and acyl chloride reagent in molar ratio: make (10～50).
The preparation method of a kind of graphene oxide ink jet recording materials of the present invention carries out according to the following steps:
One, graphite oxidation: a, take 1～8 part of graphite, 10～40 parts of strong acid, 1～5 part of nitrate, 2～100 parts of strong oxidizers and 2～8 parts of hydrogen peroxide solutions by ratio of weight and the number of copies; B, first graphite is added in the mixture of strong acid and nitrate, stir, under the mixing speed of 50～200rpm, add strong oxidizer with 50～300mg/min speed after being cooled to-5 DEG C～0 DEG C, add rear continuation and stir 24h～48h, obtain mixed liquor A; C, the mixed liquor A water-bath that step b is obtained are heated to 20 DEG C～50 DEG C and keep 40min～5h, then add 90～100 DEG C of hot water, are warming up to and seethe with excitement and keep 20min～5h, obtain mixed liquid B; Wherein the volume ratio of mixed liquor A and water is 1: (5～20); D, the hydrogen peroxide solution that step a is taken splash in the mixed liquid B that step c obtains, and stir, then filter, by solid formation washing to without SO
4 2-, then freeze drying, obtain graphite oxide;
Two, graphene oxide purifying: the graphite oxide that step 1 is obtained joins in solvent, and be placed on ultrasonator, first process duration of oscillation 0.5～12h with sonic oscillation, and then centrifugation under the condition that is 3000～10000rpm at revolution, collect upper solution, after freeze drying, obtain the graphene oxide of purifying;
Three, graphene oxide functionalization: the mol ratio of the graphene oxide of the purifying obtaining by step 2 and acyl chloride reagent is (1～5): (10～50) take graphene oxide and the acyl chloride reagent of the purifying that step 2 obtains and join in container, add anhydrous reagent, backflow 1-5h, obtains two key graphene oxides.
Four, the preparation of Graphene ink jet recording materials: take two key graphene oxides that step 3 obtains, acrylic acid, water and initator also join in reactor, wherein two key graphene oxides and acrylic acid mass ratio 1: (10～100), the quality of water is 10～50 times of acrylic acid quality, the quality of initator is 0.1～2% of acrylic acid quality, under inert gas shielding, be warming up to 50～100 DEG C and keep 0.5h～1h, obtain graphene oxide/acrylic copolymer, again graphene oxide/acrylic copolymer is coated in substrate, obtain graphene oxide ink jet recording materials.
The present invention is by after graphite oxidation, a large amount of hydroxyls and carboxyl are contained in surface, adopt chemical graft method utilization can with the material of hydroxyl or carboxyl reaction, by graphene oxide functionalization, connect two keys to graphene oxide, obtain two key-graphene oxides and carry out Raolical polymerizable and obtain copolymer with the two keys in acrylic acid, this copolymer is as the blotting material of ink absorbing layer, be attached on matrix, obtain graphene oxide ink jet recording materials.Because adhesion between the copolymer molecule as ink absorbing layer is strong, and and active force between base material and China ink grain is strong, thereby improve blotting speed, when folding, do not crack, solved fold cracks problem, production efficiency is high, this graphene oxide ink jet recording materials there is intumescent ink absorbing layer and the two advantage of air gap type ink absorbing layer.Graphene oxide ink jet recording materials has fabulous ink absorption, have glossiness like photo.
Brief description of the drawings
Fig. 1 is the stereoscan photograph of the graphene oxide ink jet recording materials section of test one preparation;
Fig. 2 is the graphene oxide ink jet recording materials light transmission photo of test one preparation;
Fig. 3 is the graphene oxide ink jet recording materials printing effect photo of test one preparation.
Detailed description of the invention
Detailed description of the invention one: a kind of graphene oxide ink jet recording materials of present embodiment is by substrate and is coated in suprabasil graphene oxide/acrylic copolymer ink absorbing layer and forms, graphene oxide/acrylic copolymer is wherein by pressing two key graphene oxides, acrylic acid, water and initiator for reaction are made, wherein two key graphene oxides and acrylic acid mass ratio 1: (10～100), the quality of water is 10～50 times of acrylic acid quality, the quality of initator is 0.1～2% of acrylic acid quality, two key graphene oxides are (1～5) by graphene oxide and acyl chloride reagent in molar ratio: make (10～50).
The graphene oxide ink jet recording materials of present embodiment, by after graphite oxidation, a large amount of hydroxyls and carboxyl are contained in surface, adopt chemical graft method utilization can with the material of hydroxyl or carboxyl reaction, by graphene oxide functionalization, connect two keys to graphene oxide, obtain two key-graphene oxides and carry out Raolical polymerizable and obtain copolymer with the two keys in acrylic acid, this copolymer, as the blotting material of ink absorbing layer, is attached on matrix, obtains Graphene ink jet recording materials.Because adhesion between the copolymer molecule as ink absorbing layer is strong, and and active force between base material and China ink grain is strong, thereby improve blotting speed, when folding, do not crack, solved fold cracks problem, production efficiency is high, this Graphene ink jet recording materials there is intumescent ink absorbing layer and the two advantage of air gap type ink absorbing layer.Graphene ink jet recording materials has fabulous ink absorption, have glossiness like photo.
Detailed description of the invention two: what present embodiment was different from detailed description of the invention one is described initiator potassium persulfate, hydrogen peroxide, water-soluble azo, benzoyl peroxide or cumyl peroxide.Other is identical with detailed description of the invention one.
Detailed description of the invention three: what present embodiment was different from detailed description of the invention one or two is that acyl chloride reagent is that acyl chloride reagent is acryloyl chloride, crotonyl chloride or prenyl chloride.Other is identical with detailed description of the invention one or two.
Detailed description of the invention four: the preparation method of a kind of graphene oxide ink jet recording materials of present embodiment carries out according to the following steps:
One, graphite oxidation: a, take 1～8 part of graphite, 10～40 parts of strong acid, 1～5 part of nitrate, 2～100 parts of strong oxidizers and 2～8 parts of hydrogen peroxide solutions by ratio of weight and the number of copies; B, first graphite is added in the mixture of strong acid and nitrate, stir, under the mixing speed of 50～200rpm, add strong oxidizer with 50～300mg/min speed after being cooled to-5 DEG C～0 DEG C, add rear continuation and stir 24h～48h, obtain mixed liquor A; C, the mixed liquor A water-bath that step b is obtained are heated to 20 DEG C～50 DEG C and keep 40min～5h, then add 90～100 DEG C of hot water, are warming up to and seethe with excitement and keep 20min～5h, obtain mixed liquid B; Wherein the volume ratio of mixed liquor A and water is 1: (5～20); D, the hydrogen peroxide solution that step a is taken splash in the mixed liquid B that step c obtains, and stir, then filter, by solid formation washing to without SO
4 2-, then freeze drying, obtain graphite oxide;
Two, graphene oxide purifying: the graphite oxide that step 1 is obtained joins in solvent, and be placed on ultrasonator, oscillation treatment 0.5～12h under the condition of ultrasonic power 100W～500W, and then centrifugation under the condition that is 3000～10000rpm at revolution, collect upper solution, after freeze drying, obtain the graphene oxide of purifying;
Three, graphene oxide functionalization: the mol ratio of the graphene oxide of the purifying obtaining by step 2 and acyl chloride reagent is (1～5): (10～50) take graphene oxide and the acyl chloride reagent of the purifying that step 2 obtains and join in container, add anhydrous solvent, backflow 1-5h, obtains two key graphene oxides.
Four, the preparation of graphene oxide ink jet recording materials: take two key graphene oxides that step 3 obtains, acrylic acid, water and initator also join in reactor, wherein two key graphene oxides and acrylic acid mass ratio 1: (10～100), the quality of water is 10～50 times of acrylic acid quality, the quality of initator is 0.1～2% of acrylic acid quality, under inert gas shielding, be warming up to 50～100 DEG C and keep 0.5h～1h, obtain graphene oxide/acrylic copolymer, again graphene oxide/acrylic copolymer is coated in substrate, obtain graphene oxide ink jet recording materials.
The graphene oxide ink jet recording materials of present embodiment, by after graphite oxidation, a large amount of hydroxyls and carboxyl are contained in surface, adopt chemical graft method utilization can with the material of hydroxyl or carboxyl reaction, by graphene oxide functionalization, connect two keys to graphene oxide, obtain two key-graphene oxides and carry out Raolical polymerizable and obtain copolymer with the two keys in acrylic acid, this copolymer, as the blotting material of ink absorbing layer, is attached on matrix, obtains Graphene ink jet recording materials.Because adhesion between the copolymer molecule as ink absorbing layer is strong, and and active force between base material and China ink grain is strong, thereby improve blotting speed, when folding, do not crack, solved fold cracks problem, production efficiency is high, this graphene oxide ink jet recording materials there is intumescent ink absorbing layer and the two advantage of air gap type ink absorbing layer.Graphene oxide ink jet recording materials has fabulous ink absorption, have glossiness like photo.
Detailed description of the invention five: the strong acid described in a of step 1 that what present embodiment was different from detailed description of the invention four is is that mass percentage concentration is the perchloric acid that >=98% the concentrated sulfuric acid or mass percentage concentration are 70%～72%; Strong oxidizer described in a of step 1 is potassium permanganate or potassium hyperchlorate; Nitrate described in a of step 1 is potassium nitrate, sodium nitrate, calcium nitrate, magnesium nitrate etc.; The mass percentage concentration of the hydrogen peroxide solution described in a of step 1 is 40%～60%.Other is identical with concrete enforcement 40.
Detailed description of the invention six: the solvent described in step 2 that what present embodiment was different from detailed description of the invention four or five is is water, ethanol, acetone, ether, chloroform, benzene, toluene, ethylene glycol, oxolane, DMF, benzinum, methyl acetate, ethyl acetate, carbon tetrachloride, pyridine, ethylenediamine or carbon disulfide.Other is identical with concrete enforcement four or five.
Detailed description of the invention seven: what present embodiment was different from one of detailed description of the invention four to six is that in step 3, acyl chloride reagent is acryloyl chloride, crotonyl chloride or prenyl chloride.Other is identical with one of concrete enforcement four to six.
Detailed description of the invention eight: what present embodiment was different from one of detailed description of the invention four to seven is that in step 3, anhydrous solvent is dimethyl sulfoxide (DMSO), oxolane or DMF.Other is identical with one of concrete enforcement four to seven.
Detailed description of the invention nine: what present embodiment was different from one of detailed description of the invention four to eight is that in step 4, initator is potassium peroxydisulfate, hydrogen peroxide, water-soluble azo, benzoyl peroxide or cumyl peroxide.Other is identical with one of concrete enforcement four to eight.
Detailed description of the invention ten: what present embodiment was different from one of detailed description of the invention four to nine is that in step 4, inert gas is nitrogen, helium or argon gas.Other is identical with one of concrete enforcement four to nine.
Detailed description of the invention 11: what present embodiment was different from one of detailed description of the invention four to ten is that in step 4, coat thickness is 1 μ m～500 μ m.Other is identical with one of concrete enforcement four to ten.
Adopt following verification experimental verification beneficial effect of the present invention:
Test one: the preparation method of the graphene oxide ink jet recording materials of this test carries out according to the following steps:
One, graphite oxidation: a, take 1 part of graphite, the 15 parts of concentrated sulfuric acid, 3 parts of sodium nitrate, 20 parts of potassium permanganate and 6 parts of hydrogen peroxide solutions that mass percentage concentration is 40% that mass percentage concentration is 98% by ratio of weight and the number of copies; B, first graphite is added in the mixture of the concentrated sulfuric acid and sodium nitrate, stir, under the mixing speed of 200rpm, add potassium permanganate with 100mg/min speed after being cooled to-2 DEG C, add rear continuation and stir 24h, obtain mixed liquor A; C, the mixed liquor A water-bath that step b is obtained are heated to 40 DEG C and keep 2h, then add 100 DEG C of hot water, are warming up to and seethe with excitement and keep 2h, obtain mixed liquid B; Wherein the volume ratio of mixed liquor A and hot water is 1: 10; D, the hydrogen peroxide solution that step a is taken splash in the mixed liquid B that step c obtains, and stir, then filter, by solid formation washing to without SO
4 2-, then freeze drying, obtain graphite oxide;
Two, graphene oxide purifying: the graphite oxide that step 1 is obtained joins in ethanol, and be placed on ultrasonator, oscillation treatment 4h under the condition of ultrasonic power 100W, and then centrifugation under the condition that is 5000rpm at revolution, collect upper solution, after freeze drying, obtain the graphene oxide of purifying;
Three, graphene oxide functionalization: the graphene oxide of the purifying obtaining by step 2 and the mol ratio of crotonyl chloride are take graphene oxide and the acyl chloride reagent of the purifying that step 2 obtains at 1: 20 and join in container, add N, dinethylformamide, backflow 4h, obtains two key graphene oxides.
Four, the preparation of graphene oxide ink jet recording materials: take two key graphene oxides that step 3 obtains, acrylic acid, water and initator also join in reactor, wherein two key graphene oxides and acrylic acid mass ratio 1: 40, the quality of water is 30 times of acrylic acid quality, the quality of initator is 1% of acrylic acid quality, under nitrogen protection, be warming up to 80 DEG C and keep 8h, obtain graphene oxide/acrylic copolymer, again graphene oxide/acrylic copolymer is coated on PET film, coat thickness is 8 μ m, obtain graphene oxide ink jet recording materials.
As shown in Figure 1, the thickness of graphene oxide/acrylic copolymer ink absorbing layer is 8 μ m to the stereoscan photograph of the graphene oxide ink jet recording materials section that this test one is obtained as can be seen from Figure 1.
The graphene oxide ink jet recording materials that this test one is obtained carries out light transmission test, and as shown in Figure 2, as can be seen from Figure 2, it is better that prepared spray is oxidized the transparency of black recording materials to the figure obtaining.
The printing effect figure of the graphene oxide ink jet recording materials that this test one is obtained as shown in Figure 3, as can be seen from Figure 3, the printing effect of graphite oxide thiazolinyl ink jet recording materials is clear, substantially not dizzy China ink occurs, proves that graphite oxide thiazolinyl ink jet recording materials has good blotting and solid performance of ink.
Claims (10)
1. a graphene oxide ink jet recording materials, it is characterized in that graphene oxide ink jet recording materials is by substrate and is coated in suprabasil graphene oxide/acrylic copolymer ink absorbing layer and forms, graphene oxide/acrylic copolymer is wherein by two key graphene oxides, acrylic acid, water and initiator for reaction are made, wherein two key graphene oxides and acrylic acid mass ratio 1:(10～100), the quality of water is 10～50 times of acrylic acid quality, the quality of initator is 0.1～2% of acrylic acid quality, two key graphene oxides are (1～5) by graphene oxide and acyl chloride reagent in molar ratio: make (10～50).
2. a kind of graphene oxide ink jet recording materials according to claim 1, is characterized in that described initator is potassium peroxydisulfate, hydrogen peroxide, water-soluble azo, benzoyl peroxide or cumyl peroxide.
3. a kind of graphene oxide ink jet recording materials according to claim 1 and 2, is characterized in that acyl chloride reagent is acryloyl chloride, crotonyl chloride or prenyl chloride.
4. the method for preparation a kind of graphene oxide ink jet recording materials as claimed in claim 1, is characterized in that the preparation method of graphene oxide ink jet recording materials carries out according to the following steps:
One, graphite oxidation: a, take 1～8 part of graphite, 10～40 parts of strong acid, 1～5 part of nitrate, 2～100 parts of strong oxidizers and 2～8 parts of hydrogen peroxide solutions by ratio of weight and the number of copies; B, first graphite is added in the mixture of strong acid and nitrate, stir, under the mixing speed of 50～200rpm, add strong oxidizer with 50～300mg/min speed after being cooled to-5 DEG C～0 DEG C, add rear continuation and stir 24h～48h, obtain mixed liquor A; C, the mixed liquor A water-bath that step b is obtained are heated to 20 DEG C～50 DEG C and keep 40min～5h, then add 90～100 DEG C of hot water, are warming up to and seethe with excitement and keep 20min～5h, obtain mixed liquid B; Wherein the volume ratio of mixed liquor A and water is 1:(5～20); D, the hydrogen peroxide solution that step a is taken splash in the mixed liquid B that step c obtains, and stir, then filter, by solid formation washing to without SO
4 2-, then freeze drying, obtain graphite oxide;
Two, graphene oxide purifying: the graphite oxide that step 1 is obtained joins in solvent, and be placed on ultrasonator, oscillation treatment 0.5～12h under the condition of ultrasonic power 100W～500W, and then centrifugation under the condition that is 3000～10000rpm at revolution, collect upper solution, after freeze drying, obtain the graphene oxide of purifying;
Three, graphene oxide functionalization: the mol ratio of the graphene oxide of the purifying obtaining by step 2 and acyl chloride reagent is (1～5): (10～50) take graphene oxide and the acyl chloride reagent of the purifying that step 2 obtains and join in container, add anhydrous solvent, backflow 1-5h, obtains two key graphene oxides;
Four, the preparation of graphene oxide ink jet recording materials: take two key graphene oxides that step 3 obtains, acrylic acid, water and initator also join in reactor, wherein two key graphene oxides and acrylic acid mass ratio 1:(10～100), the quality of water is 10～50 times of acrylic acid quality, the quality of initator is 0.1～2% of acrylic acid quality, under inert gas shielding, be warming up to 50～100 DEG C and keep 0.5h～1h, obtain graphene oxide/acrylic copolymer, again graphene oxide/acrylic copolymer is coated in substrate, obtain graphene oxide ink jet recording materials.
5. the preparation method of a kind of graphene oxide ink jet recording materials according to claim 4, is characterized in that the strong acid described in a of step 1 is that mass percentage concentration is the perchloric acid that >=98% the concentrated sulfuric acid or mass percentage concentration are 70%～72%; Strong oxidizer described in a of step 1 is potassium permanganate or potassium hyperchlorate; Nitrate described in a of step 1 is potassium nitrate, sodium nitrate, calcium nitrate, magnesium nitrate; The mass percentage concentration of the hydrogen peroxide solution described in a of step 1 is 40%～60%.
6. according to the preparation method of a kind of graphene oxide ink jet recording materials described in claim 4 or 5, it is characterized in that the solvent described in step 2 is water, ethanol, acetone, ether, chloroform, benzene, toluene, ethylene glycol, oxolane, DMF, benzinum, methyl acetate, ethyl acetate, carbon tetrachloride, pyridine, ethylenediamine or carbon disulfide.
7. according to the preparation method of a kind of graphene oxide ink jet recording materials described in claim 4 or 5, it is characterized in that in step 3, anhydrous solvent is dimethyl sulfoxide (DMSO), oxolane or DMF.
8. according to the preparation method of a kind of graphene oxide ink jet recording materials described in claim 4 or 5, it is characterized in that in step 4, initator is potassium peroxydisulfate, hydrogen peroxide, water-soluble azo, benzoyl peroxide or cumyl peroxide.
9. according to the preparation method of a kind of graphene oxide ink jet recording materials described in claim 4 or 5, it is characterized in that in step 4, inert gas is helium or argon gas.
10. according to the preparation method of a kind of graphene oxide ink jet recording materials described in claim 4 or 5, it is characterized in that in step 4, coat thickness is 1 μ m～500 μ m.
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| CN111705509A (en) * | 2020-07-08 | 2020-09-25 | 南京轮廓服饰科技有限公司 | Graphene-based lasting antibacterial composite garment fabric |
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| CN103214633B (en) * | 2013-05-02 | 2014-12-24 | 哈尔滨工业大学 | Preparation method of graphite-base flame-retardant char forming agent |
| CN107879338A (en) * | 2017-12-29 | 2018-04-06 | 天津市天波科达科技有限公司 | A kind of technical grade graphene oxide process units |
| CN110642246B (en) * | 2018-06-26 | 2021-05-28 | 中国石油天然气股份有限公司 | Preparation method of graphene microspheres |
| CN109135144B (en) * | 2018-07-11 | 2021-07-20 | 四川羽玺新材料股份有限公司 | Graphene/acrylic resin composite film and preparation method thereof |
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| CN1383401A (en) * | 2000-04-28 | 2002-12-04 | 三井化学株式会社 | Recording sheet and process for producing same |
| JP2008230206A (en) * | 2007-03-23 | 2008-10-02 | Mitsubishi Paper Mills Ltd | Inkjet recording material |
| CN102092209A (en) * | 2010-10-29 | 2011-06-15 | 哈尔滨工业大学 | Ink-jet recording material and preparation method thereof as well as method for preparing ink absorption layer coating liquid |
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| CN1383401A (en) * | 2000-04-28 | 2002-12-04 | 三井化学株式会社 | Recording sheet and process for producing same |
| JP2008230206A (en) * | 2007-03-23 | 2008-10-02 | Mitsubishi Paper Mills Ltd | Inkjet recording material |
| CN102092209A (en) * | 2010-10-29 | 2011-06-15 | 哈尔滨工业大学 | Ink-jet recording material and preparation method thereof as well as method for preparing ink absorption layer coating liquid |
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