CN109535846A - A kind of preparation method based on hydroxide radical phosphorite nanocrystalline fluorescence invisible ink - Google Patents
A kind of preparation method based on hydroxide radical phosphorite nanocrystalline fluorescence invisible ink Download PDFInfo
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- 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
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Abstract
The present invention relates to a kind of preparation method based on hydroxide radical phosphorite nanocrystalline fluorescence invisible ink, soluble calcium salt, which is dissolved in deionized water, forms solution A；Soluble citrate and amino acid, which are dissolved in deionized water, forms solution B；Soluble phosphate, which is dissolved in deionized water, forms solution C；Solution B is added drop-wise in solution A, and stirring forms mixed liquor one；Solution C is added drop-wise in mixed liquor one, and stirring forms mixed liquor two；The heating reaction of mixed liquor two, it is centrifugated after cooling, sediment deionized water and dehydrated alcohol alternating centrifugal wash, it is scattered in deionized water again, up to the nanocrystalline dispersion liquid of water soluble hydroxy apatite fluorescent, water soluble hydroxy apatite fluorescent nano-crystalline granule mass fraction, pH value are in adjusting dispersion liquid to get fluorescence invisible ink.Raw material sources of the present invention are abundant, and synthesis technology is simple；For product in colourless under natural light, fluorescence invisible ink issues visible light under ultraviolet light, is suitable for writings, inkjet printing, seal mark etc..
Description
Technical field
It is especially a kind of based on the ultraviolet of hydroxyapatite nanoparticle the present invention relates to colorless fluorescent invisible ink field
The preparation method of fluorescence invisible ink.
Background technique
Anti-counterfeiting ink is for the needs such as product false proof, vital document be anti-fake, to concealed anti-false label, text, image etc.
Content carries out the ink of printing.Fluorescence invisible ink has implementation process simple, at low cost, good concealment, and reproducibility is strong, examines
The features such as easy is surveyed, is widely applied in fields such as bank note, bill, stamps as one of important anti-counterfeiting mark.
The country has certain research achievement to fluorescence invisible ink at present, but mostly with organic fluorescent dye or organic dilute
Earth metal fluorescent complex is as fluorescence radiation agent, and with certain toxicity, environmentally friendly index is low, understands body to people and generates bad shadow
It rings.And the domestic research for being suitable for the fluorescent ink of inkjet printing also stays at foundation phase.
CN108624150A discloses a kind of fluorescence falsification preventing coding ink, based on parts by weight, including nitrocotton, asphalt mixtures modified by epoxy resin
Rouge, solvent type fluorescent dye, fluorescent powder, organic solvent, polyoxethylene octylphenyl phenol ether part and N-Methyl pyrrolidone；It is described molten
Dosage form fluorescent dye is selected from one or more of orange red fluorescence, fluorescein and phloxine.
Hydroxyapatite has very excellent bioactivity and biocompatibility, is widely used to Bone Defect Repari, bone replaces
The fields such as generation and pharmaceutical carrier.Since hydroxyapatite itself is unstressed configuration property, achieving photoluminescent property at present is mainly,
Replaced by expensive rare earth elements europium or terbium to realize no matter do not make us from preparation cost or biocompatibility angle
It is satisfied.
So far, few without relying on the case of rear-earth-doped fluorescence hydroxide radical phosphorite nanocrystalline, it especially can be with
The hydroxyl apatite fluorescent ink for being applied to inkjet printing has not been reported.Therefore, a kind of superior colloidal stability is developed, and glimmering
The high undoped hydroxyl apatite fluorescent ink of luminous intensity, and can apply it in ink-jet printer just has very strong reality to anticipate
Justice.
Summary of the invention
The purpose of the present invention is intended to provide one kind under natural light in colourless, the base of sending visible light under ultraviolet light
In the fluorescence invisible ink of hydroxide radical phosphorite nanocrystalline.
The implementation of the object of the invention is a kind of system based on water soluble hydroxy phosphorite nanocrystalline fluorescence invisible ink
Preparation Method, the specific steps are as follows:
1) 0.01mol soluble calcium salt is dissolved in 10 grams of deionized waters, forms solution A；
The soluble calcium salt is calcium nitrate or calcium chloride；
2) 0.003-0.02mol soluble citrate and 0.001-0.01mol soluble amino acid are dissolved in 10 grams
In ionized water, solution B is formed；
The soluble citrate is sodium citrate or potassium citrate；
The soluble amino acid is nor-leucine or arginine；
3) 0.006mol soluble phosphate is dissolved in 15 grams of deionized waters, forms solution C；
The soluble phosphate is sodium phosphate, disodium hydrogen phosphate, potassium phosphate or dipotassium hydrogen phosphate；
4) step 2) acquired solution B is added dropwise in step 1) acquired solution A at room temperature, 15min, shape is sufficiently stirred
At mixed liquor one；
5) step 3) acquired solution C is added dropwise in mixed liquor one obtained by step 4) at room temperature, is sufficiently stirred
15min forms mixed liquor two；
6) mixed liquor two obtained by step 5) is transferred in closed hydrothermal reactor, it is small that 1-12 is reacted at 120-200 DEG C
Shi Hou, cooled to room temperature obtain reaction solution；
7) reaction solution obtained by step 6) is centrifugated using supercentrifuge, obtains sediment, sediment using go from
Three times, excessive electrolyte, is then scattered in deionized water again in removal system for sub- water and the washing of dehydrated alcohol alternating centrifugal,
Up to the nanocrystalline dispersion liquid of water soluble hydroxy apatite fluorescent；Adjust hydroxyl in the nanocrystalline dispersion liquid of water soluble hydroxy apatite fluorescent
Base apatite fluorescent nano-crystalline granule mass concentration is 0.1-50wt%, adjusts water-soluble hydroxyl using the sodium hydroxide solution of 0.1M
The nanocrystalline dispersion liquid pH to 8.0-10.0 of base apatite fluorescent is to get based on hydroxide radical phosphorite nanocrystalline fluorescence invisible ink.
The invention has the advantages that raw material is that nontoxic green, abundance is easy to get, is low in cost；Synthesis technology is simple, easy
In implementation；Gained is based on hydroxide radical phosphorite nanocrystalline fluorescence invisible ink quality stabilization and good process repeatability.
Hydroxide radical phosphorite nanocrystalline fluorescence invisible ink good dispersion produced by the present invention, in colourless under natural light,
Visible light is issued under ultraviolet light, fluorescence intensity is high, can be used as anti-fake material application, is suitable for writing, inkjet printing, seal
Marking etc..
Detailed description of the invention
Fig. 1 is the X-ray diffractogram of the water soluble fluorescence hydroxide radical phosphorite nanocrystalline of embodiment 1,
Fig. 2 is the transmission electron microscope photo of the water soluble fluorescence hydroxide radical phosphorite nanocrystalline of embodiment 1,
Fig. 3 is the dynamic light scattering diagram of the water soluble fluorescence hydroxide radical phosphorite nanocrystalline of embodiment 1,
Fig. 4 is the fluorescent exciting of water soluble fluorescence hydroxide radical phosphorite nanocrystalline prepared by embodiment 1 and comparative example 1
Spectrogram.
Fig. 5 is the fluorescence emission of water soluble fluorescence hydroxide radical phosphorite nanocrystalline prepared by embodiment 1 and comparative example 1
Spectrogram.
Fig. 6 a, b are the texts for the fluorescence invisible ink writing that hydroxide radical phosphorite nanocrystalline is prepared in embodiment 1 in nature
Comparison diagram is irradiated under light and ultraviolet light.
Specific embodiment
Soluble calcium salt is dissolved in deionized water by the present invention forms solution A；Soluble citrate and amino acid is molten
Solution B is formed in deionized water；Soluble phosphate is dissolved in deionized water and forms solution C；At room temperature dropwise by solution B
It is added in solution A, stirring forms mixed liquor one；Solution C is added dropwise in mixed liquor one, and stirring forms mixed liquor two；Mixed liquor
Two in closed hydrothermal reactor, reacts at 120-200 DEG C, is centrifugated after cooling, sediment deionized water and anhydrous second
The washing of alcohol alternating centrifugal, is scattered in deionized water again to get the nanocrystalline dispersion liquid of water soluble hydroxy apatite fluorescent.Adjust water
The nanocrystalline dispersion particle mass concentration of soluble hydroxy apatite fluorescent is 0.1-50wt%, utilizes the sodium hydroxide solution of 0.1M
The nanocrystalline dispersion liquid pH to 8.0-10.0 of water soluble hydroxy apatite fluorescent is adjusted to get hydroxide radical phosphorite nanocrystalline fluorescence is based on
Invisible ink.
The nanocrystalline average diameter of the water soluble hydroxy apatite fluorescent is 10-30nm, average length 50-200nm.
Hydroxide radical phosphorite nanocrystalline fluorescence invisible ink is bright colourless dispersion liquid, is swashed under 360nm length ultraviolet light
Issue blue-fluorescence.Suitable for writing, inkjet printing, seal marking etc..
The present invention is described in detail with specific embodiment below.
Experimental method used in following embodiments is conventional method unless otherwise specified.
The materials, reagents and the like used in the following examples is commercially available unless otherwise specified.
Embodiment 1,
1) 0.01mol calcium chloride is dissolved in 10 grams of deionized waters, forms solution A；
2) 0.015mol sodium citrate and 0.007mol arginine are dissolved in 10 grams of deionized waters, form solution B；
3) 0.006mol disodium hydrogen phosphate is dissolved in 15 grams of deionized waters, forms solution C；
4) step 2) acquired solution B is added dropwise in step 1) acquired solution A at room temperature, 15min, shape is sufficiently stirred
At mixed liquor one；
5) step 3) acquired solution C is added dropwise in mixed liquor one obtained by step 4) at room temperature, is sufficiently stirred
15min forms mixed liquor two；
6) mixed liquor two obtained by step 5) is transferred in closed hydrothermal reactor, after being reacted 3 hours at 190 DEG C, from
It is so cooled to room temperature, obtains reaction solution；
7) reaction solution obtained by step 6) is centrifugated using supercentrifuge, obtains sediment, sediment using go from
Three times, excessive electrolyte, is then scattered in deionized water again in removal system for sub- water and the washing of dehydrated alcohol alternating centrifugal,
Up to the nanocrystalline dispersion liquid of water soluble hydroxy apatite fluorescent, hydroxyl apatite fluorescent nano-crystalline granule quality in dispersion liquid is adjusted
Concentration is 10wt%, adjusts dispersion liquid pH to 9.5 using the sodium hydroxide solution of 0.1M to get hydroxide radical phosphorite nanocrystalline fluorescence
Invisible ink.
The X-ray diffractogram of the water soluble fluorescence hydroxide radical phosphorite nanocrystalline is shown in Fig. 1, it can be seen from figure 1 that product crystal phase is
Pure ha phase, no other miscellaneous phases exist, and crystallinity is good.
Transmission electron microscope photo is shown in Fig. 2, and water soluble fluorescence hydroxide radical phosphorite nanocrystalline is Rod-like shape as seen from Figure 2, puts down
Equal diameter is about 10-30nm, average length 50-200nm.
Dynamic light scattering diagram is shown in Fig. 3, as can be seen from Figure 3 the aquation dynamics of water soluble fluorescence hydroxide radical phosphorite nanocrystalline
Radius is 124.6nm, and polydispersity 0.17, particle zeta potential value is -44.6mV, and dispersion liquid is apparently clear, colorless
Shape illustrates it with splendid water dispersible.
Embodiment 2: with embodiment 1, the difference is that,
1) 0.01mol calcium nitrate is dissolved in 10 grams of deionized waters, forms solution A；
2) 0.003mol potassium citrate and 0.001mol nor-leucine are dissolved in 10 grams of deionized waters, form solution B；
3) 0.006mol potassium phosphate is dissolved in 15 grams of deionized waters, forms solution C；
6) mixed liquor two obtained by step 5) is transferred in closed hydrothermal reactor, after being reacted 12 hours at 120 DEG C, from
It is so cooled to room temperature, obtains reaction solution；
7) step 6) reaction solution is centrifugally separating to obtain sediment using supercentrifuge, sediment using deionized water and
Dehydrated alcohol alternating centrifugal washs three times, and excessive electrolyte, is then scattered in deionized water again in removal system, adjusts and divides
Dispersion liquid particle mass concentration is 0.1wt%, adjusts dispersion liquid pH to 8.0 using the sodium hydroxide solution of 0.1M to get hydroxyl phosphorus
The nanocrystalline fluorescence invisible ink of lime stone.
Embodiment 3, with embodiment 1, the difference is that,
2) 0.006mol sodium citrate and 0.003mol arginine are dissolved in 10 grams of deionized waters, form solution B；
3) 0.006mol dipotassium hydrogen phosphate is dissolved in 15 grams of deionized waters, forms solution C；
6) mixed liquor two obtained by step 5) is transferred in closed hydrothermal reactor, after being reacted 9 hours at 150 DEG C, from
It is so cooled to room temperature, obtains reaction solution；
7) reaction solution obtained by step 6) is centrifugated using supercentrifuge, obtains sediment, sediment using go from
Three times, excessive electrolyte, is then scattered in deionized water again in removal system for sub- water and the washing of dehydrated alcohol alternating centrifugal,
Adjusting dispersion particle mass concentration is 5wt%, adjusts dispersion liquid pH to 8.5 using the sodium hydroxide solution of 0.1M to get hydroxyl
Base phosphorite nanocrystalline fluorescence invisible ink.
Embodiment 4, with embodiment 1, the difference is that,
1) 0.01mol calcium chloride is dissolved in 10 grams of deionized waters, forms solution A；
2) 0.01mol sodium citrate and 0.005mol arginine are dissolved in 10 grams of deionized waters, form solution B；
3) 0.006mol sodium phosphate is dissolved in 15 grams of deionized waters, forms solution C；
6) mixed liquor two obtained by step 5) is transferred in closed hydrothermal reactor, after being reacted 6 hours at 180 DEG C, from
It is so cooled to room temperature, obtains reaction solution；
7) reaction solution obtained by step 6) is centrifugally separating to obtain sediment using supercentrifuge, sediment utilizes deionization
Three times, excessive electrolyte, is then scattered in deionized water again in removal system, adjusts for water and the washing of dehydrated alcohol alternating centrifugal
Section dispersion particle mass concentration is 20wt%, adjusts dispersion liquid pH to 9.0 using the sodium hydroxide solution of 0.1M to get hydroxyl
Phosphorite nanocrystalline fluorescence invisible ink.
Embodiment 5, with embodiment 1, the difference is that,
2) 0.02mol potassium citrate and 0.01mol arginine are dissolved in 10 grams of deionized waters, form solution B；
3) 0.006mol sodium phosphate is dissolved in 15 grams of deionized waters, forms solution C；
6) mixed liquor two obtained by step 5) is transferred in closed hydrothermal reactor, after being reacted 1 hour at 200 DEG C, from
It is so cooled to room temperature, obtains reaction solution；
7) reaction solution obtained by step 6) is centrifugated using supercentrifuge, obtains sediment, sediment using go from
Three times, excessive electrolyte, is then scattered in deionized water again in removal system for sub- water and the washing of dehydrated alcohol alternating centrifugal,
Adjusting dispersion particle mass concentration be 50wt%, using 0.1M sodium hydroxide solution adjust dispersion liquid pH to 10.0 to get
Hydroxide radical phosphorite nanocrystalline fluorescence invisible ink.
To confirm effect of the invention, the applicant spy has made following comparative example.
Comparative example 1:
1) 0.01mol calcium chloride is dissolved in 10 grams of deionized waters, forms solution A；
2) 0.01mol sodium citrate is dissolved in 10 grams of deionized waters, forms solution B；
3) 0.006mol sodium phosphate is dissolved in 15 grams of deionized waters, forms solution C；
4) step 2) acquired solution B is added dropwise in step 1) acquired solution A at room temperature, 15min, shape is sufficiently stirred
At mixed liquor one；
5) step 3) acquired solution C is added dropwise in mixed liquor one obtained by step 4) at room temperature, is sufficiently stirred
15min forms mixed liquor two；
6) mixed liquor two obtained by step 5) is transferred in closed hydrothermal reactor, after being reacted 6 hours at 180 DEG C, from
It is so cooled to room temperature, obtains reaction solution；
7) it is centrifuged reaction solution obtained by step 6) to obtain sediment using supercentrifuge, utilizes deionized water and anhydrous second
Alcohol alternating centrifugal washs 3 times, and excessive electrolyte, is then scattered in deionized water again in removal system, adjusts dispersion liquid
Grain mass concentration is 10wt%, adjusts dispersion liquid pH to 9.0 using the sodium hydroxide solution of 0.1M to get hydroxyapatite nano
Brilliant fluorescence invisible ink, gained hydroxide radical phosphorite nanocrystalline fluorescence invisible ink is without obvious photoluminescent property.
Comparative example 2:
1) 0.01mol calcium chloride is dissolved in 10 grams of deionized waters, forms solution A；
2) 0.01mol sodium citrate and 0.05mol arginine are dissolved in 10 grams of deionized waters, form solution B；
3) 0.006mol sodium phosphate is dissolved in 15 grams of deionized waters, forms solution C；
4) step 2) acquired solution B is added dropwise in step 1) acquired solution A at room temperature, 15min, shape is sufficiently stirred
At mixed liquor one；
5) step 3) acquired solution C is added dropwise in mixed liquor one obtained by step 4) at room temperature, is sufficiently stirred
15min forms mixed liquor two；
6) mixed liquor two obtained by step 5) is transferred in closed hydrothermal reactor, after being reacted 0.5 hour at 90 DEG C, from
It is so cooled to room temperature, obtains reaction solution；
7) it is centrifuged reaction solution obtained by step 6) to obtain sediment using supercentrifuge, utilizes deionized water and anhydrous second
Alcohol alternating centrifugal washs 3 times, and excessive electrolyte, is then scattered in deionized water again in removal system, adjusts dispersion liquid
Grain mass concentration is 15wt%, adjusts dispersion liquid pH to 9.0 using the sodium hydroxide solution of 0.1M to get hydroxyapatite nano
Brilliant fluorescence invisible ink, gained hydroxide radical phosphorite nanocrystalline fluorescence invisible ink is without obvious photoluminescent property.
Comparative example 1 is compared with embodiment 4, does not add arginine in step 2), comparative example 2 and embodiment 4 compare, and step 2) adds
Arginine, but step 6) reacted 0.5 hour at 90 DEG C, reaction temperature are lower than 90 DEG C, and the reaction time is lower than 1 hour, i.e.,
Lower than temperature of the invention, the lower limit value in reaction time.
Fig. 4 and Fig. 5 is the water solubility of the water soluble fluorescence hydroxide radical phosphorite nanocrystalline and comparative example 1 in embodiment 1
The fluorescence excitation spectrum and emission spectrum of hydroxide radical phosphorite nanocrystalline illustrate that the water soluble hydroxy apatite of comparative example 1 is received
The obvious fluorescence excitation peak of meter Jing Wu and fluorescence emission peak, reason is that step 2) does not add arginine, and the water solubility of embodiment 1 is glimmering
Light hydroxide radical phosphorite nanocrystalline has a very strong fluorescence excitation peak near 365nm, while having near 440nm one very strong
Fluorescence emission peak.Arginine is not added and is that no primary amine group causes without obvious fluorescence excitation peak and the reason of fluorescence emission peak
Citrate molecule between dehydration condensation.
With 1 gained hydroxyl apatite fluorescent ink of embodiment write text can not with the naked eye recognize under visible light (see
Fig. 6 a), and write text is clear that under ultraviolet excitation (see Fig. 6 b).
Comparative example 2 is lower than temperature of the invention, the lower limit in reaction time because of the reaction temperature of step 6), reaction time
Value, can not effectively carry out dehydration condensation, therefore gained hydroxide radical phosphorite nanocrystalline fluorescence invisible ink is without obvious photoluminescent property.
Claims (3)
1. a kind of preparation method based on hydroxide radical phosphorite nanocrystalline fluorescence invisible ink, it is characterised in that: specific step is as follows:
1) 0.01mol soluble calcium salt is dissolved in 10 grams of deionized waters, forms solution A；
The soluble calcium salt is calcium nitrate or calcium chloride；
2) 0.003-0.02mol soluble citrate and 0.001-0.01mol soluble amino acid are dissolved in 10 grams of deionizations
In water, solution B is formed；
The soluble citrate is sodium citrate or potassium citrate；
The soluble amino acid is nor-leucine or arginine；
3) 0.006mol soluble phosphate is dissolved in 15 grams of deionized waters, forms solution C；
The soluble phosphate is sodium phosphate, disodium hydrogen phosphate, potassium phosphate or dipotassium hydrogen phosphate；
4) step 2) acquired solution B is added dropwise in step 1) acquired solution A at room temperature, 15min is sufficiently stirred, formed mixed
Close liquid one；
5) step 3) acquired solution C is added dropwise in mixed liquor one obtained by step 4) at room temperature, 15min, shape is sufficiently stirred
At mixed liquor two；
6) mixed liquor two obtained by step 5) is transferred in closed hydrothermal reactor, after being reacted 1-12 hours at 120-200 DEG C,
Cooled to room temperature obtains reaction solution；
7) reaction solution obtained by step 6) is centrifugated using supercentrifuge, obtains sediment, sediment utilizes deionized water
With dehydrated alcohol alternating centrifugal washing three times, excessive electrolyte in removal system, be then scattered in again in deionized water to get
The nanocrystalline dispersion liquid of water soluble hydroxy apatite fluorescent；Adjust hydroxyl phosphorus in the nanocrystalline dispersion liquid of water soluble hydroxy apatite fluorescent
Lime stone fluorescence nano particle mass concentration is 0.1-50wt%, adjusts water soluble hydroxy phosphorus using the sodium hydroxide solution of 0.1M
Lime stone fluorescence nano dispersion liquid pH to 8.0-10.0 is to get based on hydroxide radical phosphorite nanocrystalline fluorescence invisible ink.
2. a kind of preparation method based on hydroxide radical phosphorite nanocrystalline fluorescence invisible ink according to claim 1, special
Sign is: the resulting nanocrystalline diameter of water soluble hydroxy apatite fluorescent of step 7) is 10-30nm, long 50-200nm.
3. a kind of preparation method based on hydroxide radical phosphorite nanocrystalline fluorescence invisible ink according to claim 1, special
Sign is: step 7) gained is bright colourless dispersion liquid based on hydroxyl apatite fluorescent invisible ink, is issued under ultraviolet light
Blue-fluorescence.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115521218A (en) * | 2022-07-26 | 2022-12-27 | 盐城工学院 | Preparation method of amino acid surfactant raw material |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105722784A (en) * | 2013-09-10 | 2016-06-29 | 巴黎高等物理化工学院 | Nanoparticles for use in bioadhesion |
| CN105885529A (en) * | 2016-05-06 | 2016-08-24 | 安徽雅美油墨有限公司 | Modified water-based polyurethane ink containing nano-hydroxyapatite and preparation method of modified water-based polyurethane ink |
| CN107758638A (en) * | 2017-11-14 | 2018-03-06 | 湖北工业大学 | A kind of nanocrystalline preparation method of water soluble hydroxy apatite fluorescent |
| CN107778991A (en) * | 2017-11-02 | 2018-03-09 | 武汉理工大学 | One kind is without zirconium ultrawhite inkjet printing aqueous ceramic ink and preparation method thereof |
-
2018
- 2018-12-21 CN CN201811572997.2A patent/CN109535846A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105722784A (en) * | 2013-09-10 | 2016-06-29 | 巴黎高等物理化工学院 | Nanoparticles for use in bioadhesion |
| CN105885529A (en) * | 2016-05-06 | 2016-08-24 | 安徽雅美油墨有限公司 | Modified water-based polyurethane ink containing nano-hydroxyapatite and preparation method of modified water-based polyurethane ink |
| CN107778991A (en) * | 2017-11-02 | 2018-03-09 | 武汉理工大学 | One kind is without zirconium ultrawhite inkjet printing aqueous ceramic ink and preparation method thereof |
| CN107758638A (en) * | 2017-11-14 | 2018-03-06 | 湖北工业大学 | A kind of nanocrystalline preparation method of water soluble hydroxy apatite fluorescent |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115521218A (en) * | 2022-07-26 | 2022-12-27 | 盐城工学院 | Preparation method of amino acid surfactant raw material |
| CN115521218B (en) * | 2022-07-26 | 2023-08-22 | 盐城工学院 | Preparation method of amino acid surfactant raw material |
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