CN110385045B - Efficient desalting method in preparation process of digital ink-jet ink - Google Patents
Efficient desalting method in preparation process of digital ink-jet ink Download PDFInfo
- Publication number
- CN110385045B CN110385045B CN201910618359.8A CN201910618359A CN110385045B CN 110385045 B CN110385045 B CN 110385045B CN 201910618359 A CN201910618359 A CN 201910618359A CN 110385045 B CN110385045 B CN 110385045B
- Authority
- CN
- China
- Prior art keywords
- nanospheres
- cellulose acetate
- ink
- prepare
- desalting
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/02—Reverse osmosis; Hyperfiltration ; Nanofiltration
- B01D61/027—Nanofiltration
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0002—Organic membrane manufacture
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/08—Polysaccharides
- B01D71/12—Cellulose derivatives
- B01D71/14—Esters of organic acids
- B01D71/16—Cellulose acetate
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/38—Polyalkenylalcohols; Polyalkenylesters; Polyalkenylethers; Polyalkenylaldehydes; Polyalkenylketones; Polyalkenylacetals; Polyalkenylketals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/40—Polymers of unsaturated acids or derivatives thereof, e.g. salts, amides, imides, nitriles, anhydrides, esters
- B01D71/42—Polymers of nitriles, e.g. polyacrylonitrile
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
- Y02A20/124—Water desalination
- Y02A20/131—Reverse-osmosis
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Water Supply & Treatment (AREA)
- Life Sciences & Earth Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
- Ink Jet Recording Methods And Recording Media Thereof (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention discloses a high-efficiency desalting method in a preparation process of digital ink-jet ink, which comprises the following steps: firstly, preparing cellulose acetate nanospheres, then preparing the silicon oxide coated cellulose acetate nanospheres by adopting a sol-gel method, adding the silicon oxide coated cellulose acetate nanospheres into a polyethylene glycol solution, and reacting polyethylene glycol adsorbed on the surfaces of the nanospheres with methacrylic acid and acrylamide under a certain condition to prepare modified nanospheres; and finally, adding a Tris-HCl buffer solution containing dopamine hydrochloride into a tea saponin mixed solution, adding modified nanospheres to prepare a dispersion solution, depositing the dispersion solution on the surface of a polyacrylonitrile nanofiltration membrane to form a hydrophilic layer to prepare a hydrophilic nanofilm, adding the hydrophilic nanofilm into a nanofilter provided with a hydrophilic nanofiltration membrane, and performing desalting treatment to prepare the low-salinity digital inkjet ink. The method is simple to operate, and the adopted nanofiltration membrane has excellent pollution resistance and good desalting effect.
Description
The technical field is as follows:
the invention relates to a desalting process for ink preparation, in particular to a high-efficiency desalting method in a preparation process of digital ink-jet ink.
Background art:
the membrane pollution is a main problem of good and bad desalting treatment effect in the ink preparation process, and is also one of the key points of attention of researchers in the membrane technical field for many years. The membrane pollution refers to the phenomenon that pollutants are accumulated on the membrane surface or in membrane pores, and can bring about a plurality of serious consequences, such as low production efficiency caused by reduced membrane flux after the membrane pollution occurs, and the membrane pollution can only be maintained in a mode of improving operation pressure and increasing operation energy consumption; membrane fouling may alter the ability of the membrane to retain the contaminants, thereby making the resulting dye ink of poor quality. Therefore, the preparation of the anti-pollution high-flux nanofiltration membrane is a key problem in the ink desalting process.
The physicochemical properties of the membrane affecting membrane fouling include membrane material, hydrophilicity and hydrophobicity of the membrane surface, electric charge, water molecular state of the membrane surface, surface free energy, membrane pore size and porosity, surface roughness and the like. The physicochemical properties of the contaminants including the hydrophilicity and hydrophobicity, charge, size, shape, water molecular state on the surface of the contaminants, etc. also have an important influence on membrane fouling. Membrane fouling is also directly related to the physicochemical properties of the feed liquid to be separated. The properties mainly comprise the properties, composition, concentration, particle size distribution, viscosity, pH value and the like of each component of the mixed solution. The pollution degree of membranes made of different materials caused by adhesion and pore blockage is different, membrane materials such as polyethylene, polyvinylidene fluoride, polyether sulfone, polysulfone and polyacrylonitrile have strong hydrophobicity, so that pollutants are irreversibly adsorbed on the surface of the membrane to cause serious membrane pollution, and hydrophilic cellulosic membranes cause relatively light pollution. Charged membranes suffer from more severe membrane fouling than neutral membranes, since many contaminants are charged in the feed solution and tend to be electrostatically adsorbed on the membrane surface to form membrane fouling. The operating conditions of membrane separation, including operating pressure, temperature, membrane surface tangential flow velocity, hydraulic residence time, etc., also have a significant impact on membrane fouling. The flow velocity of the feed liquid is improved, the shearing effect of the feed liquid on the membrane surface is greatly improved, the concentration polarization can be reduced, and the water flux is improved.
The invention content is as follows:
the invention aims to provide a high-efficiency desalting method in the preparation process of digital ink-jet ink aiming at the defects of the prior art, the method can effectively remove inorganic salt and other small molecules in dye molecules, and the prepared ink has good stability, less pollution of a nano-filtration membrane, reusability and high desalting efficiency.
In order to achieve the purpose, the invention adopts the following technical scheme:
a high-efficiency desalting method in the preparation process of digital ink-jet ink comprises the following steps:
(1) dissolving cellulose acetate in a mixed solution of ethyl acetate and ethanol in a volume ratio of 1:1, then adding a sodium carbonate aqueous solution with a mass concentration of 10%, continuously adding a polyvinyl alcohol aqueous solution with a mass concentration of 0.15% after uniformly mixing, stirring and uniformly mixing, removing an organic solvent, and drying to obtain cellulose acetate nanospheres;
(2) dispersing the cellulose acetate nanospheres prepared in the step (1) in deionized water to prepare dispersion liquid; dissolving ethyl orthosilicate in ethanol, adding the prepared dispersion, stirring at normal temperature for reaction for 4-9h, filtering after the reaction is finished, precipitating, washing with deionized water, and drying to obtain silicon oxide-coated cellulose acetate nanospheres;
(3) adding the silicon oxide-coated cellulose acetate nanospheres into a 3% polyethylene glycol aqueous solution, then dropwise adding the aqueous solution into a mixed monomer emulsion of methacrylic acid and acrylamide, adding triethanolamine serving as a catalyst, stirring and reacting at 60 ℃ for 5 hours, cooling to room temperature after the reaction is finished, filtering, precipitating and drying to obtain modified nanospheres;
(4) dissolving dopamine hydrochloride in a Tris-HCl buffer solution, adding an ethanol/deionized water mixed solution containing tea saponin, adding the prepared modified nanospheres, uniformly stirring and mixing to prepare a dispersion liquid, spraying the dispersion liquid on the surface of a clean polyacrylonitrile nanofiltration membrane, and drying to form a hydrophilic layer to prepare the hydrophilic nanofiltration membrane;
(5) performing membrane desalting treatment under the conditions of water bath circulation at 25 +/-5 ℃ and pressure of 1MPa, adding 18 mass percent of acid red 18-containing ink-jet ink into a nanofiltration device provided with the prepared hydrophilic nanofiltration membrane for pre-circulation for 1h before desalting, timing and sampling every time when the volume of penetrating fluid is 2L, adding 2L of distilled water into the nanofiltration device after sampling to keep the volume of feed liquid unchanged, and performing circulating desalting treatment to prepare the low-salinity ink-jet ink.
Preferably, in the step (1), the mass ratio of the cellulose acetate, the sodium carbonate and the polyvinyl alcohol is 5: (0.13-0.16): 0.2.
preferably, in the step (1), the cellulose acetate nanospheres have a diameter of 50-60 nm.
Preferably, in the step (2), the mass ratio of the cellulose acetate nanospheres to the tetraethoxysilane is 3: (4-9).
Preferably, in the step (3), the mass ratio of the silicon oxide-coated cellulose acetate nanospheres, the polyethylene glycol, the methacrylic acid, the acrylamide and the triethanolamine is 2: 0.15: (3-5): 1: 001.
preferably, in the step (4), the Tris-HCl buffer solution has a molar concentration of 10mmol/L and a pH of 7.
Preferably, in the step (4), the mass ratio of the dopamine hydrochloride, the tea saponin and the modified nanospheres is 1: 0.03: (1-4).
Preferably, in the step (4), in the hydrophilic nanofiltration membrane, the thickness of the hydrophilic layer is 10-20 nm.
Preferably, in the step (5), the inkjet ink is composed of, by mass, 18% of acid red 18 dye molecules, 10% of ethanol, 1% of sodium dodecyl benzene sulfonate, 3% of propylene glycol, 0.55% of triethanolamine, and 67.45% of deionized water.
Compared with the prior art, the invention has the following advantages:
the method is used for improving the desalting effect in the preparation of the ink-jet ink by preparing the nanofiltration membrane with excellent pollution resistance and hydrophilicity; firstly, taking cellulose acetate as a raw material to prepare cellulose acetate nanospheres, wherein the surfaces of the cellulose acetate nanospheres have a porous structure and a plurality of active sites, then adding the cellulose acetate nanospheres into an ethanol solution containing tetraethoxysilane to prepare silicon oxide coated cellulose acetate nanospheres, in order to further improve the dispersibility of the silicon oxide coated cellulose acetate nanospheres, firstly adding the cellulose acetate nanospheres into a water solution of polyethylene glycol to activate the surfaces of the silicon oxide coated cellulose acetate nanospheres, then adding the silicon oxide coated cellulose acetate nanospheres into a mixed emulsion of methacrylic acid and acrylamide, grafting the methacrylic acid and the acrylamide onto the surfaces of the silicon oxide coated cellulose acetate nanospheres under the action of triethanolamine to prepare modified nanospheres, adding the modified nanospheres into tea saponin for dissolution, adding a Tris-HCl buffer solution containing dopamine hydrochloride, and adsorbing the dopamine hydrochloride onto the surfaces of the modified nanospheres, when the modified nanosphere is sprayed on the surface of polyacrylonitrile, dopamine hydrochloride forms a self-assembly layer on the surface of the polyacrylonitrile, the modified nanospheres are uniformly attached to the surface of a membrane to form a hydrophilic layer, the compactness of polymer chain segments is damaged to a certain extent by the modified nanospheres, the looseness of the polyacrylonitrile can be effectively improved, and the permeability of a nanofiltration membrane is improved.
The specific implementation mode is as follows:
in order to better understand the present invention, the following examples further illustrate the invention, the examples are only used for explaining the invention, not to constitute any limitation of the invention.
Methacrylic acid: analytical grade, Tianjin Kowei Chemicals, Inc.
Ethyl orthosilicate: analytical grade, Tianjin Kowei Chemicals, Inc.
Polyethylene glycol: chemical purity, tianjinke wafer chemicals ltd.
Cellulose acetate: degree of substitution Ds 2.45, Nantong acetate fiber, Inc.
Polyvinyl alcohol: the polymerization degree is 1700, the alcoholysis degree is 88 percent, and the product is produced by a Sichuan vinylon factory.
Example 1
A high-efficiency desalting method in the preparation process of digital ink-jet ink comprises the following steps:
(1) dissolving cellulose acetate in a mixed solution of ethyl acetate and ethanol in a volume ratio of 1:1, adding a sodium carbonate aqueous solution with a mass concentration of 10%, uniformly mixing, continuously adding a polyvinyl alcohol aqueous solution with a mass concentration of 0.15%, uniformly stirring and mixing, removing an organic solvent, and drying to obtain cellulose acetate nanospheres with the particle size of 50-60 nm; wherein the mass ratio of the cellulose acetate to the sodium carbonate to the polyvinyl alcohol is 5: 0.13: 0.2;
(2) dispersing the prepared cellulose acetate nanospheres in deionized water to prepare dispersion liquid; dissolving ethyl orthosilicate in ethanol, adding the prepared dispersion, stirring and reacting for 4 hours at normal temperature, filtering after the reaction is finished, washing precipitates by deionized water, and drying to prepare silicon oxide coated cellulose acetate nanospheres; wherein the mass ratio of the cellulose acetate nanospheres to the ethyl orthosilicate is 3: 4;
(3) adding the silicon oxide-coated cellulose acetate nanospheres into a 3% polyethylene glycol aqueous solution, then dropwise adding the aqueous solution into a mixed monomer emulsion of methacrylic acid and acrylamide, adding triethanolamine serving as a catalyst, stirring at 60 ℃ for reaction for 5 hours, cooling to room temperature after the reaction is finished, filtering, precipitating and drying to obtain modified nanospheres, wherein the mass ratio of the silicon oxide-coated cellulose acetate nanospheres to the polyethylene glycol to the methacrylic acid to the acrylamide to the triethanolamine is 2: 0.15: 3: 1: 001;
(4) dissolving dopamine hydrochloride in Tris-HCl buffer solution, adding ethanol/deionized water mixed solution of tea saponin, adding the prepared modified nanospheres, stirring and mixing uniformly to prepare dispersion liquid, and spraying the dispersion liquid on the surface of a cleaned polyacrylonitrile nanofiltration membrane for drying treatment to form a hydrophilic layer with the thickness of 10-20 nm; preparing a hydrophilic nanofiltration membrane; wherein the mass ratio of the dopamine hydrochloride to the tea saponin to the modified nanospheres is 1: 0.03: 1;
(5) performing membrane desalting treatment under the conditions of water bath circulation at 25 +/-5 ℃ and 1MPa of pressure, adding 18 mass percent of acid red ink-jet ink into a nanofiltration device provided with the prepared hydrophilic nanofiltration membrane for pre-circulation for 1h before desalting, timing and sampling every time when the volume of penetrating fluid is 2L, adding 2L of distilled water into the nanofiltration device after sampling to keep the volume of feed liquid unchanged, and performing circulating desalting treatment to prepare low-salinity ink-jet ink; the ink-jet ink comprises, by mass, 18% of acid red 18 dye molecules, 10% of ethanol, 1% of sodium dodecyl benzene sulfonate, 3% of propylene glycol, 0.55% of triethanolamine and 67.45% of deionized water.
Example 2
A high-efficiency desalting method in the preparation process of digital ink-jet ink comprises the following steps:
(1) dissolving cellulose acetate in a mixed solution of ethyl acetate and ethanol in a volume ratio of 1:1, adding a sodium carbonate aqueous solution with a mass concentration of 10%, uniformly mixing, continuously adding a polyvinyl alcohol aqueous solution with a mass concentration of 0.15%, uniformly stirring and mixing, removing an organic solvent, and drying to obtain cellulose acetate nanospheres with the particle size of 50-60 nm; wherein the mass ratio of the cellulose acetate to the sodium carbonate to the polyvinyl alcohol is 5: 0.16: 0.2;
(2) dispersing the prepared cellulose acetate nanospheres in deionized water to prepare dispersion liquid; dissolving ethyl orthosilicate in ethanol, adding the prepared dispersion, stirring and reacting for 9 hours at normal temperature, filtering after the reaction is finished, washing precipitates by deionized water, and drying to prepare silicon oxide coated cellulose acetate nanospheres; wherein the mass ratio of the cellulose acetate nanospheres to the ethyl orthosilicate is 3: 9;
(3) adding the cellulose acetate nanospheres coated with silicon oxide into a polyethylene glycol aqueous solution with the mass concentration of 3%, then dropwise adding mixed monomer emulsion of methacrylic acid and acrylamide, adding triethanolamine serving as a catalyst, stirring at 60 ℃ for reaction for 5 hours, cooling to room temperature after the reaction is finished, filtering, precipitating and drying to obtain modified nanospheres, wherein the mass ratio of the cellulose acetate nanospheres coated with silicon oxide to the polyethylene glycol to the methacrylic acid to the acrylamide to the triethanolamine is 2: 0.15: 5: 1: 001;
(4) dissolving dopamine hydrochloride in Tris-HCl buffer solution, adding ethanol/deionized water mixed solution of tea saponin, adding the prepared modified nanospheres, stirring and mixing uniformly to prepare dispersion liquid, and spraying the dispersion liquid on the surface of a cleaned polyacrylonitrile nanofiltration membrane for drying treatment to form a hydrophilic layer with the thickness of 10-20 nm; preparing a hydrophilic nanofiltration membrane; wherein the mass ratio of the dopamine hydrochloride to the tea saponin to the modified nanospheres is 1: 0.03: 4;
(5) performing membrane desalting treatment under the conditions of water bath circulation at 25 +/-5 ℃ and 1MPa of pressure, adding 18 mass percent of acid red ink-jet ink into a nanofiltration device provided with the prepared hydrophilic nanofiltration membrane for pre-circulation for 1h before desalting, timing and sampling every time when the volume of penetrating fluid is 2L, adding 2L of distilled water into the nanofiltration device after sampling to keep the volume of feed liquid unchanged, and performing circulating desalting treatment to prepare low-salinity ink-jet ink; the ink-jet ink comprises, by mass, 18% of acid red 18 dye molecules, 10% of ethanol, 1% of sodium dodecyl benzene sulfonate, 3% of propylene glycol, 0.55% of triethanolamine and 67.45% of deionized water.
Example 3
A high-efficiency desalting method in the preparation process of digital ink-jet ink comprises the following steps:
(1) dissolving cellulose acetate in a mixed solution of ethyl acetate and ethanol in a volume ratio of 1:1, adding a sodium carbonate aqueous solution with a mass concentration of 10%, uniformly mixing, continuously adding a polyvinyl alcohol aqueous solution with a mass concentration of 0.15%, uniformly stirring and mixing, removing an organic solvent, and drying to obtain cellulose acetate nanospheres with the particle size of 50-60 nm; wherein the mass ratio of the cellulose acetate to the sodium carbonate to the polyvinyl alcohol is 5: 0.14: 0.2;
(2) dispersing the prepared cellulose acetate nanospheres in deionized water to prepare dispersion liquid; dissolving ethyl orthosilicate in ethanol, adding the prepared dispersion, stirring and reacting for 5 hours at normal temperature, filtering after the reaction is finished, washing precipitates by deionized water, and drying to prepare silicon oxide coated cellulose acetate nanospheres; wherein the mass ratio of the cellulose acetate nanospheres to the ethyl orthosilicate is 3: 5;
(3) adding the silicon oxide-coated cellulose acetate nanospheres into a 3% polyethylene glycol aqueous solution, then dropwise adding a mixed monomer emulsion of methacrylic acid and acrylamide, adding triethanolamine serving as a catalyst, stirring at 60 ℃ for reaction for 5 hours, cooling to room temperature after the reaction is finished, filtering, precipitating and drying to obtain modified nanospheres; wherein, the mass ratio of the silicon oxide-coated cellulose acetate nanospheres, the polyethylene glycol, the methacrylic acid, the acrylamide and the triethanolamine is 2: 0.15: 3.5: 1: 001;
(4) dissolving dopamine hydrochloride in a Tris-HCl buffer solution, adding an ethanol/deionized water mixed solution of tea saponin, adding the prepared modified nanospheres, uniformly stirring and mixing to prepare a dispersion liquid, spraying the dispersion liquid on the surface of a cleaned polyacrylonitrile nanofiltration membrane, and drying to form a hydrophilic layer with the thickness of 10-20nm to prepare the hydrophilic nanofiltration membrane; wherein the mass ratio of the dopamine hydrochloride to the tea saponin to the modified nanospheres is 1: 0.03: 2;
(5) performing membrane desalting treatment under the conditions of water bath circulation at 25 +/-5 ℃ and 1MPa of pressure, adding 18 mass percent of acid red ink-jet ink into a nanofiltration device provided with the prepared hydrophilic nanofiltration membrane for pre-circulation for 1h before desalting, timing and sampling every time when the volume of penetrating fluid is 2L, adding 2L of distilled water into the nanofiltration device after sampling to keep the volume of feed liquid unchanged, and performing circulating desalting treatment to prepare low-salinity ink-jet ink; the ink-jet ink comprises, by mass, 18% of acid red 18 dye molecules, 10% of ethanol, 1% of sodium dodecyl benzene sulfonate, 3% of propylene glycol, 0.55% of triethanolamine and 67.45% of deionized water.
Example 4
A high-efficiency desalting method in the preparation process of digital ink-jet ink comprises the following steps:
(1) dissolving cellulose acetate in a mixed solution of ethyl acetate and ethanol in a volume ratio of 1:1, adding a sodium carbonate aqueous solution with a mass concentration of 10%, uniformly mixing, continuously adding a polyvinyl alcohol aqueous solution with a mass concentration of 0.15%, uniformly stirring and mixing, removing an organic solvent, and drying to obtain cellulose acetate nanospheres with the particle size of 50-60 nm; wherein the mass ratio of the cellulose acetate to the sodium carbonate to the polyvinyl alcohol is 5: 0.145: 0.2;
(2) dispersing the prepared cellulose acetate nanospheres in deionized water to prepare dispersion liquid; dissolving ethyl orthosilicate in ethanol, adding the prepared dispersion, stirring and reacting for 6 hours at normal temperature, filtering after the reaction is finished, washing precipitates by deionized water, and drying to prepare silicon oxide coated cellulose acetate nanospheres; wherein the mass ratio of the cellulose acetate nanospheres to the ethyl orthosilicate is 3: 5;
(3) adding the silicon oxide-coated cellulose acetate nanospheres into a 3% polyethylene glycol aqueous solution, then dropwise adding a mixed monomer emulsion of methacrylic acid and acrylamide, adding triethanolamine serving as a catalyst, stirring at 60 ℃ for reaction for 5 hours, cooling to room temperature after the reaction is finished, filtering, precipitating and drying to obtain modified nanospheres; wherein, the mass ratio of the silicon oxide-coated cellulose acetate nanospheres, the polyethylene glycol, the methacrylic acid, the acrylamide and the triethanolamine is 2: 0.15: 4: 1: 001;
(4) dissolving dopamine hydrochloride in a Tris-HCl buffer solution, adding an ethanol/deionized water mixed solution of tea saponin, adding the prepared modified nanospheres, uniformly stirring and mixing to prepare a dispersion liquid, spraying the dispersion liquid on the surface of a cleaned polyacrylonitrile nanofiltration membrane, and drying to form a hydrophilic layer with the thickness of 10-20nm to prepare the hydrophilic nanofiltration membrane; wherein the mass ratio of the dopamine hydrochloride to the tea saponin to the modified nanospheres is 1: 0.03: 2.5;
(5) performing membrane desalting treatment under the conditions of water bath circulation at 25 +/-5 ℃ and 1MPa of pressure, adding 18 mass percent of acid red ink-jet ink into a nanofiltration device provided with the prepared hydrophilic nanofiltration membrane for pre-circulation for 1h before desalting, timing and sampling every time when the volume of penetrating fluid is 2L, adding 2L of distilled water into the nanofiltration device after sampling to keep the volume of feed liquid unchanged, and performing circulating desalting treatment to prepare low-salinity ink-jet ink; the ink-jet ink comprises, by mass, 18% of acid red 18 dye molecules, 10% of ethanol, 1% of sodium dodecyl benzene sulfonate, 3% of propylene glycol, 0.55% of triethanolamine and 67.45% of deionized water.
Example 5
A high-efficiency desalting method in the preparation process of digital ink-jet ink comprises the following steps:
(1) dissolving cellulose acetate in a mixed solution of ethyl acetate and ethanol in a volume ratio of 1:1, adding a sodium carbonate aqueous solution with a mass concentration of 10%, uniformly mixing, continuously adding a polyvinyl alcohol aqueous solution with a mass concentration of 0.15%, uniformly stirring and mixing, removing an organic solvent, and drying to obtain cellulose acetate nanospheres with the particle size of 50-60 nm; wherein the mass ratio of the cellulose acetate to the sodium carbonate to the polyvinyl alcohol is 5: 0.15: 0.2;
(2) dispersing the prepared cellulose acetate nanospheres in deionized water to prepare dispersion liquid; dissolving ethyl orthosilicate in ethanol, adding the prepared dispersion, stirring and reacting for 7 hours at normal temperature, filtering after the reaction is finished, washing precipitates by deionized water, and drying to prepare silicon oxide coated cellulose acetate nanospheres; wherein the mass ratio of the cellulose acetate nanospheres to the ethyl orthosilicate is 3: 5;
(3) adding the silicon oxide-coated cellulose acetate nanospheres into a 3% polyethylene glycol aqueous solution, then dropwise adding a mixed monomer emulsion of methacrylic acid and acrylamide, adding triethanolamine serving as a catalyst, stirring at 60 ℃ for reaction for 5 hours, cooling to room temperature after the reaction is finished, filtering, precipitating and drying to obtain modified nanospheres; wherein, the mass ratio of the silicon oxide-coated cellulose acetate nanospheres, the polyethylene glycol, the methacrylic acid, the acrylamide and the triethanolamine is 2: 0.15: 4: 1: 001;
(4) dissolving dopamine hydrochloride in a Tris-HCl buffer solution, adding an ethanol/deionized water mixed solution of tea saponin, adding the prepared modified nanospheres, uniformly stirring and mixing to prepare a dispersion liquid, spraying the dispersion liquid on the surface of a cleaned polyacrylonitrile nanofiltration membrane, and drying to form a hydrophilic layer with the thickness of 10-20nm to prepare the hydrophilic nanofiltration membrane; wherein the mass ratio of the dopamine hydrochloride to the tea saponin to the modified nanospheres is 1: 0.03: 3.5;
(5) performing membrane desalting treatment under the conditions of water bath circulation at 25 +/-5 ℃ and 1MPa of pressure, adding 18 mass percent of acid red ink-jet ink into a nanofiltration device provided with the prepared hydrophilic nanofiltration membrane for pre-circulation for 1h before desalting, timing and sampling every time when the volume of penetrating fluid is 2L, adding 2L of distilled water into the nanofiltration device after sampling to keep the volume of feed liquid unchanged, and performing circulating desalting treatment to prepare low-salinity ink-jet ink; the ink-jet ink comprises, by mass, 18% of acid red 18 dye molecules, 10% of ethanol, 1% of sodium dodecyl benzene sulfonate, 3% of propylene glycol, 0.55% of triethanolamine and 67.45% of deionized water.
The concentration of chloride ions in the ink-jet ink adopted by the invention is 0.55mol/L, the molar concentration of sulfate ions is 0.24mol/L, the volume of the ink-jet ink is 10L, and the inorganic salt treatment effect and the anti-pollution performance of the nanofiltration membrane are tested.
The concentrations of chloride ions and sulfate ions in the inkjet ink after the desalting treatment were measured, and the inorganic salt removal rate was characterized according to the change in the inorganic salt ion concentration before and after the treatment, and the measurement results are shown in table 1:
TABLE 1
From the test results, the desalting method disclosed by the invention not only can effectively remove chloride ions in the ink-jet ink, but also has a good effect of removing sulfate ions.
The pure water flux of the hydrophilic nanofiltration membrane is tested after the hydrophilic nanofiltration membrane is treated by the ink-jet ink for 10 hours, and the anti-pollution performance of the hydrophilic nanofiltration membrane is represented according to the difference of the pure water flux between the front and the back. The test results are shown in table 2.
TABLE 2
From the test results, the pure water flux of the hydrophilic nanofiltration membrane adopted by the invention is reduced less after the membrane desalination treatment, and the pollution resistance is excellent.
Although specific embodiments of the invention have been described, many other forms and modifications of the invention will be apparent to those skilled in the art. It is to be understood that the appended claims and this invention generally cover all such obvious forms and modifications which are within the true spirit and scope of the present invention.
Claims (7)
1. A high-efficiency desalting method in the preparation process of digital ink-jet ink is characterized by comprising the following steps:
(1) dissolving cellulose acetate in a mixed solution of ethyl acetate and ethanol in a volume ratio of 1:1, then adding a sodium carbonate aqueous solution with a mass concentration of 10%, continuously adding a polyvinyl alcohol aqueous solution with a mass concentration of 0.15% after uniformly mixing, stirring and uniformly mixing, removing an organic solvent, and drying to obtain cellulose acetate nanospheres;
(2) dispersing the cellulose acetate nanospheres prepared in the step (1) in deionized water to prepare dispersion liquid; dissolving ethyl orthosilicate in ethanol, adding the prepared dispersion, stirring at normal temperature for reaction for 4-9h, filtering after the reaction is finished, precipitating, washing with deionized water, and drying to obtain silicon oxide-coated cellulose acetate nanospheres;
(3) adding the silicon oxide-coated cellulose acetate nanospheres into a 3% polyethylene glycol aqueous solution, then dropwise adding the aqueous solution into a mixed monomer emulsion of methacrylic acid and acrylamide, adding triethanolamine serving as a catalyst, stirring and reacting at 60 ℃ for 5 hours, cooling to room temperature after the reaction is finished, filtering, precipitating and drying to obtain modified nanospheres;
(4) dissolving dopamine hydrochloride in a Tris-HCl buffer solution, adding an ethanol/deionized water mixed solution containing tea saponin, adding the prepared modified nanospheres, uniformly stirring and mixing to prepare a dispersion liquid, spraying the dispersion liquid on the surface of a clean polyacrylonitrile nanofiltration membrane, and drying to form a hydrophilic layer to prepare the hydrophilic nanofiltration membrane;
(5) performing membrane desalting treatment under the conditions of water bath circulation at 25 +/-5 ℃ and pressure of 1MPa, adding the ink-jet ink containing 18 mass percent of acid red 18 into a nanofiltration device provided with the prepared hydrophilic nanofiltration membrane for pre-circulation for 1h, timing and sampling every time when the volume of penetrating fluid is 2L, adding 2L of distilled water into the nanofiltration device after sampling to keep the volume of feed liquid unchanged, and performing circulating desalting treatment to prepare the low-salinity ink-jet ink.
2. The method for removing salt efficiently in the preparation process of digital ink-jet ink according to claim 1, wherein in the step (1), the mass ratio of the cellulose acetate, the sodium carbonate and the polyvinyl alcohol is 5: (0.13-0.16): 0.2.
3. the method for efficient desalting in the preparation of digital inkjet ink according to claim 1, wherein in the step (1), the cellulose acetate nanospheres have a diameter of 50-60 nm.
4. The method for efficient desalting in the preparation process of digital inkjet ink according to claim 1, wherein in the step (2), the mass ratio of the cellulose acetate nanospheres to the ethyl orthosilicate is 3: (4-9).
5. The method for efficient desalting in the preparation of digital ink-jet ink according to claim 1, wherein in the step (4), the Tris-HCl buffer solution has a molar concentration of 10mmol/L and a pH of 7.
6. The method for removing salt efficiently in the preparation process of digital inkjet ink according to claim 1, wherein in the step (4), the mass ratio of the dopamine hydrochloride, the tea saponin and the modified nanospheres is 1: 0.03: (1-4).
7. The method for efficient desalting in the preparation process of digital inkjet ink according to claim 1, wherein in the step (5), the inkjet ink comprises 18% of acid red 18 dye molecules, 10% of ethanol, 1% of sodium dodecyl benzene sulfonate, 3% of propylene glycol, 0.55% of triethanolamine, and 67.45% of deionized water by mass percent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910618359.8A CN110385045B (en) | 2019-07-10 | 2019-07-10 | Efficient desalting method in preparation process of digital ink-jet ink |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910618359.8A CN110385045B (en) | 2019-07-10 | 2019-07-10 | Efficient desalting method in preparation process of digital ink-jet ink |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110385045A CN110385045A (en) | 2019-10-29 |
| CN110385045B true CN110385045B (en) | 2021-08-10 |
Family
ID=68286386
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910618359.8A Active CN110385045B (en) | 2019-07-10 | 2019-07-10 | Efficient desalting method in preparation process of digital ink-jet ink |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110385045B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117025024B (en) * | 2023-10-09 | 2024-01-02 | 山东概念印刷有限公司 | Water-based ink composition for flexographic printing and preparation method thereof |
Family Cites Families (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102311505B (en) * | 2011-07-18 | 2012-12-05 | 东华大学 | Method for preparing cellulose nanospheres based on waste dissolvable fibers |
| CN102443314A (en) * | 2011-10-26 | 2012-05-09 | 日冠(福建)针纺织机械有限公司 | Cold dyeing digital direct injection printing ink and its application technology |
| TW201351758A (en) * | 2012-06-11 | 2013-12-16 | Enerage Inc | Isolation film of electrochemical device and manufacturing method thereof |
| CN102925002B (en) * | 2012-11-27 | 2014-07-16 | 江南大学 | Preparation method of white paint ink used for textile inkjet printing |
| GB201304770D0 (en) * | 2013-03-15 | 2013-05-01 | Provost Fellows Foundation Scholars And The Other Members Of Board Of | A scalable process for producing exfoliated defect-free, non-oxidised 2-dimens ional materials in large quantities |
| CN103265710B (en) * | 2013-05-20 | 2014-10-15 | 东华大学 | Micro/nano sphere preparation method |
| CN103418250B (en) * | 2013-07-05 | 2015-12-02 | 烟台绿水赋膜材料有限公司 | A kind of method at separation membrane surface in-situ preparation nano particle |
| CN103464013B (en) * | 2013-07-25 | 2014-11-05 | 烟台绿水赋膜材料有限公司 | High-performance hybrid separation membrane and preparation method thereof |
| CN103566776B (en) * | 2013-11-06 | 2015-06-17 | 复旦大学 | Photocatalytic inorganic nanoparticle/polydopamine/polymer self-cleaning composite film and preparation method thereof |
| SG10202008907TA (en) * | 2014-10-03 | 2020-10-29 | Univ Rice William M | Use of surface modified porous membranes for fluid distillation |
| KR20160123187A (en) * | 2015-04-15 | 2016-10-25 | 한국화학연구원 | Nanocomposite ultrafiltration membrane containing graphene oxide or reduced graphene oxide and preparation method thereof |
| CN105879701B (en) * | 2016-05-06 | 2018-09-25 | 北京林业大学 | A kind of NEW TYPE OF COMPOSITE forward osmosis membrane of two-dimension nano materials inlay and preparation method thereof |
| CN106582298A (en) * | 2016-12-09 | 2017-04-26 | 西安建筑科技大学 | Three-dimensional GO sheet sphere particle modified organic composite ultra/micro filtering membrane preparing method |
| CN106861470B (en) * | 2017-03-31 | 2019-06-28 | 东北林业大学 | A kind of preparation method of coated with silica charcoal enhancing ethanol selectivity infiltrating and vaporizing membrane |
| CN107513375B (en) * | 2017-08-11 | 2021-06-01 | 中科世宇(北京)科技有限公司 | Phase-change microcapsule coated with silicon dioxide and preparation method and application thereof |
| CN107469653B (en) * | 2017-08-16 | 2019-12-31 | 江苏大学 | Synthesis method of molecular imprinting composite membrane for enriching and separating norfloxacin |
| CN109972421A (en) * | 2019-04-22 | 2019-07-05 | 浙江海印数码科技有限公司 | A kind of reactive dye ink and preparation method thereof suitable for ultrahigh speed digital printing |
-
2019
- 2019-07-10 CN CN201910618359.8A patent/CN110385045B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN110385045A (en) | 2019-10-29 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| WO2018120476A1 (en) | Supramolecular composite nano-filtration membrane and preparation method therefor and use thereof | |
| CN110339726B (en) | Polystyrene microsphere/carbon nanotube composite modified hybrid polyethersulfone nanofiltration membrane as well as preparation method and application thereof | |
| CN103464004B (en) | high-strength nano modified ultrafiltration membrane and preparation method thereof | |
| CN102085459B (en) | Preparation method of anti-pollution oil-water separation ultrafiltration membrane | |
| CN110841487B (en) | Preparation method of seawater desalination membrane | |
| CN105617882A (en) | Chitosan modified graphene oxide nano composite positive osmotic membrane and preparation method thereof | |
| CN104607056A (en) | Hollow fiber compound nanofiltration membrane and preparation method thereof | |
| CN102580561B (en) | Tubular composite nanofiltration membrane | |
| CN111085119B (en) | Modified separation membrane for membrane distillation and preparation method and application thereof | |
| CN109304088A (en) | A kind of sea water desalination membrane of strong alkali-acid resistance and the preparation method and application thereof | |
| CN103861480A (en) | Preparation method of hydrophilic polyvinylidene fluoride flat sheet membrane and hollow fiber membrane | |
| CN104028120A (en) | Method for preparing carboxymethylcellulose sodium composite-filled polyamide nanofiltration membrane | |
| CN106512729A (en) | High-desalinization-rate reverse osmosis composite membrane and preparing method thereof | |
| CN110813103A (en) | Preparation method of antibacterial and anti-pollution hollow fiber membrane | |
| CN108744994A (en) | A kind of preparation method of high throughput anti-pollution NF membrane | |
| CN110385045B (en) | Efficient desalting method in preparation process of digital ink-jet ink | |
| CN112604507A (en) | Preparation method of high-flux dye separation nanofiltration membrane | |
| CN110359298B (en) | Preparation method of low-salinization reactive dye and application of low-salinization reactive dye in ink-jet printing ink | |
| CN108325390A (en) | A method of improving the compound film properties of polyethyleneimine/sodium lignin sulfonate | |
| CN107376667B (en) | Method and device for preparing nano-filtration/forward-osmosis amphibious-performance CTA (CTA) membrane | |
| CN108479414B (en) | Hollow fiber polymer membrane, preparation method and application thereof in brine refining | |
| CN110270235A (en) | The composite nanometer filtering film that a kind of pair of monovalence, divalent salts efficiently separate | |
| CN110743383B (en) | Modification method for improving permeation flux of polyamide composite membrane | |
| CN116143234A (en) | Preparation method of sea water desalination reverse osmosis membrane and reverse osmosis membrane prepared by same | |
| CN116371221B (en) | Polyamide nanofiltration membrane and preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20230109 Address after: 522 (4), Floor 5, Building 1, Yard 178, Binhe Road, Miyun District, Beijing 101500 Patentee after: Beijing Jingjun Technology Co.,Ltd. Address before: 312000 west side of the first floor of building 4 on the west side of Linhai Road, Yuecheng District, Shaoxing City, Zhejiang Province Patentee before: Zhejiang Haiyin Digital Technology Co.,Ltd. |
|
| TR01 | Transfer of patent right |