CN108660852A - A kind of preparation method and products thereof of stress induction type paper false proof coating - Google Patents
A kind of preparation method and products thereof of stress induction type paper false proof coating Download PDFInfo
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- CN108660852A CN108660852A CN201810378753.4A CN201810378753A CN108660852A CN 108660852 A CN108660852 A CN 108660852A CN 201810378753 A CN201810378753 A CN 201810378753A CN 108660852 A CN108660852 A CN 108660852A
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H19/00—Coated paper; Coating material
- D21H19/36—Coatings with pigments
- D21H19/38—Coatings with pigments characterised by the pigments
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/102—Metallic powder coated with organic material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H19/00—Coated paper; Coating material
- D21H19/36—Coatings with pigments
- D21H19/44—Coatings with pigments characterised by the other ingredients, e.g. the binder or dispersing agent
- D21H19/46—Non-macromolecular organic compounds
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H19/00—Coated paper; Coating material
- D21H19/36—Coatings with pigments
- D21H19/44—Coatings with pigments characterised by the other ingredients, e.g. the binder or dispersing agent
- D21H19/46—Non-macromolecular organic compounds
- D21H19/48—Diolefins, e.g. butadiene; Aromatic vinyl monomers, e.g. styrene; Polymerisable unsaturated acids or derivatives thereof, e.g. acrylic acid
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
- D21H21/14—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by function or properties in or on the paper
- D21H21/16—Sizing or water-repelling agents
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
- D21H21/14—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by function or properties in or on the paper
- D21H21/40—Agents facilitating proof of genuineness or preventing fraudulent alteration, e.g. for security paper
- D21H21/44—Latent security elements, i.e. detectable or becoming apparent only by use of special verification or tampering devices or methods
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Physics & Mathematics (AREA)
- Composite Materials (AREA)
- Inorganic Chemistry (AREA)
- General Physics & Mathematics (AREA)
- Materials Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Paper (AREA)
Abstract
The present invention provides a kind of preparation methods of stress induction type paper false proof coating：（1）By HAuCl4It is boiled after being dissolved in water with PVP DADMAN, reducing agent is then added, be protected from light and be stirred to react, modified Nano gold particle is obtained after centrifuged supernatant vacuum drying；（2）PEOS is diluted in ASA, as oil phase；By step（1）The modified Nano gold of preparation is soluble in water, and it is acidity to adjust pH, as water phase；By water phase and oil phase, ultrasonic wave stirs in a heated condition, and the Pickering lotions of oil-in-water type ASA, i.e. stress induction type paper false proof coating are obtained after standing.The present invention can get the Pickering lotions of stable oil-in-water type ASA, the coalescence between ASA oil droplets can be effectively reduced, stability of emulsion is greatly improved, the emulsion-stabilizing several months is precipitated without water phase and oil phase, and need not add any surfactant and other modifying agent.
Description
Technical field
A kind of application field that the invention belongs to nano materials in papermaking, and in particular to alkenyl succinic acid of stress induction
Acid anhydride（ASA）The technology of preparing of paper false proof lotion.
Background technology
Anti-counterfeit paint can be applied in commodity packaging and Trademark design, to prevent product to be counterfeited infringement, be given birth to for product
Production person, consumer and dealer provide the powerful measure of a differentiation commodity true and false.The application of anti-counterfeit paint typically is provided with down
State condition：Discoloration has invertibity, and the irritability such as triggering discoloration at normal temperatures become colour-stable, accurate, distinct, general without weight
Metal, toxic object and mordant acid and alkali substance.Anti-counterfeit paint cannot be used as general merchandise to launch into market,
One enterprise generally should have anti-counterfeit paint the manufacturing right or the right to use of monopoly, and this requires work out more multi items and performance
Anti-counterfeit paint, to meet the needs of more different commodity.Be generally basede on camouflage paint development anti-counterfeit paint can only be it at the beginning of
Step application and function, however the developing direction of anti-counterfeit paint and antiforge agent should be will vary with temperature, intensity of illumination, pH become
Change, changes of magnetic field or other changing factors and change colour, alternating temperature etc. causes the anti-forgery inks of inductance characteristics, for printing the quotient of product
Mark and specification etc..The variation of anti-counterfeit paint tone at present has substantial connection with ambient humidity, in the case where humidity is very low, i.e.,
Make not heat, coating may also lose the crystallization water and change colour.When ambient humidity is larger, it may be necessary to just may be used at relatively high temperatures
It is to seal film when being normally applied currently in order to preventing the influence of ambient humidity to lose the variation of the crystallization water and display color
It closes.This just needs a kind of anti-counterfeit paint technology of preparing of hydrophobic to make up this limitation.
Invention content
For current ambient humidity is influenced on anti-counterfeit paint the problems such as big, the present invention provides a kind of alkenyls of stress induction
Succinic anhydride（ASA）The preparation method of anti-counterfeit paint need not add other surfaces activating agent, and the anti-counterfeit paint of acquisition is to humidity
Stability is good.
To achieve the above object, the present invention adopts the following technical scheme that.
A kind of preparation method of stress induction type paper false proof coating, includes the following steps：
（1）By HAuCl4（Tetra chlorauric acid）And PVP-DADMAN（It is poly-（Diallydimethyl-ammonium nitrate）Ethenyl pyrrolidone
Ketone）It is boiled after being dissolved in water, reducing agent is then added, be protected from light and be stirred to react, obtaining modification after centrifuged supernatant vacuum drying receives
Rice gold particle；
（2）By PEOS（Polyethoxy siloxanes）It is diluted in ASA（Alkenyl succinic anhydride）In, as oil phase；By step（1）It prepares
Modified Nano gold it is soluble in water, adjust pH be acidity, as water phase；By water phase and oil phase, ultrasonic wave stirs in a heated condition
It mixes, the Pickering lotions of oil-in-water type ASA, i.e. stress induction type paper false proof coating is obtained after standing.
The weight average molecular weight M of the PVP-DADMANwFor 55-68kg/mol, more preferably 60kg/mol.
The HAuCl4Mass ratio with PVP-DADMAN is 60:1-20:1, preferably 35:1.The HAuCl4Concentration
Preferably 1 × 10-2-1×10-4M, more preferably 3 × 10-3M；The concentration of the PVP-DADMAN is preferably 1 × 10-7-1×10-5M, more preferably 6 × 10-6M。
The reducing agent is selected from ascorbic acid or thiocarbamide；Preferably ascorbic acid.
The HAuCl4Mass ratio with reducing agent is 3:1-1:5, preferably 1:2.
Step（1）In, the boiling time is 1h；The temperature of reduction reaction is 98 DEG C, reaction time 1h；Centrifugal speed
For 5000-20000rpm, centrifugation time 5-30min.
Step（1）In, the shape of the modified Nano gold particle is nearly hexagon；Average grain diameter is 15-65nm, preferably
30-45nm。
The weight average molecular weight M of the PEOSwFor 1-3kg/mol, more preferably 1.3kg/mol.
Step（2）In, the mass ratio of the PEOS and ASA are 1:3-1:10；More preferably 1:6.
Step（2）In, the mass ratio of the PEOS and modified Nano gold is 1:2-5:1, preferably 2:1.
Step（2）In, the mass percentage concentration of the modified Nano gold solution is 0.4%-1.2%.
Step（2）In, the pH is 1-4；Preferably 2.The acid of pH is adjusted to be inorganic acid or organic acid；It preferably is selected from
Hydrochloric acid or citric acid.
Step（2）In, the volume ratio of the oil phase and water phase is 1:5-1:1, preferably 1:2.Oil phase is mixed with water can
Can also be that oil phase is added in water phase to be that water phase is added in oil phase；Preferably water phase is added in oil phase.
Step（2）In, heating temperature is 65 DEG C -80 DEG C；Preferably 70 DEG C.The time of repose is 2-5 days.
A kind of paper using above-mentioned stress induction type paper false proof coating preparation.
Pass through PVP-DADMAN and HAuCl in the present invention4Reduction reaction is carried out by diallydimethyl-ammonium nitrate long bone
Frame is grafted on a nanometer gold surface, is modified to nanogold, improves its lipophile；Then modified Nano gold is embedded by PEOS
On, its oleophylic performance is further increased, it can further affine ASA.The modification for by adjusting pH value PEOS being embedded
Nanogold charge repulsion reduces, and forms bulk emulsifier particle that is fine and close, stablizing, wraps up ASA, form stable
Pickering lotions.
The present invention has the following advantages：
The present invention can be effective by the diallydimethyl in PVP-DADMAN-ammonium nitrate long bone bridge joint branch and PEOS embeddings
Improve the lipophile of gold nano grain；The Pickering lotions of acquisition have the three-phase contact angle close to 90 °, and zeta current potentials are about
It is 0；The Pickering lotions for obtaining stable oil-in-water type ASA, can effectively reduce the coalescence between ASA oil droplets, substantially
Stability of emulsion is improved, the emulsion-stabilizing several months is precipitated without water phase and oil phase, and need not add any surfactant and its
His modifying agent, step are simple, easy to operate.
Description of the drawings
Fig. 1 is the transmission electron microscope picture of modified Nano gold particle；
Fig. 2 is the Pickering lotion microscope photographs of ASA.
Specific implementation mode
With reference to embodiment, the present invention will be further described with attached drawing, but the present invention is not limited by following embodiments
System.
Embodiment 1
（1）By the HAuCl of 60 parts by weight4With the M of 1 parts by weightwIt is dissolved in water respectively for the PVP-DADMAN of 68kg/mol, obtains dense
Degree is 1 × 10-2The HAuCl of M4Solution and a concentration of 5 × 10-6The solution of the PVP-DADMAN of M boils 1h after mixing, then add
Enter the ascorbic acid of 50 parts by weight, 98 DEG C are protected from light and are stirred to react 1h, after 8000rpm centrifuges 15min supernatant；By supernatant
Modified Nano gold particle, average grain diameter 65nm are obtained after vacuum drying；
（2）By the M of 1 parts by weightwIt is dissolved in the ASA of 3 parts by weight for the PEOS of 1kg/mol, as oil phase；By step（1）It prepares
Modified Nano gold take 2 parts by weight to be dispersed in water, be made mass percentage concentration be 0.4% solution, be added dropwise dilute hydrochloric acid adjust pH
To 1, as water phase；Water phase is added in oil phase, the volume ratio of oil phase and water phase is 1:5, at room temperature ultrasonic wave stir 15min,
The Pickering lotions of oil-in-water type ASA, i.e. ASA paper false proofs coating, the average grain of sizing agent emulsion are obtained after standing 2 days
Diameter is 1.8 μm, and lotion placement is unchanged for 24 hours, has good stability.
The sized paper performance test of ASA paper false proof coating：
Hydrophobic anti-counterfeiting performance：The paper of test first carries out top sizing by ASA paper false proofs coating, and sizing agent dosage is 8 ‰
（Ratios of the ASA relative to absolute dried paper pulp, similarly hereinafter）, sized paper surface is in light blue, and top sizing degree is 1427 seconds（GB/T
5405-2002）, with 162 ° of water contact angle, belong to super hydrophobic surface.
Strain induction anti-counterfeiting performance：Induction is stretched, sized paper is placed on transparent glass surface, paper is clamped with pliers
And slowly pulled, the color change of sized paper is observed with light microscope, with the stretching of paper, film color is from light
Blue gradually becomes pink colour, eventually becomes red；Mechanical force impact induction up and horizontal spreads the sizing of sized paper
Exhibition takes the iron block of 200g weights to be suspended from above sized paper, carries out free-falling according to different height and falls to sized paper
On, changing for the sized paper color after being impacted by iron block is observed and recorded with light microscope, with iron block height of drop
It gradually rises, is showed light blue, pink colour, lavender and red respectively by the shock point position of the sized paper of iron block impact
Variation；Perforation induction, the paper being glued to ASA paper false proof coating with paper puncher carry out mechanical force punching, bore hole device to hole
It is observed in hole, it can be seen that sized paper perforated edge will present out different colors, from the distant to the near apart from hole edge
Color change is：Light blue, pale pink, pink colour, lavender and red.
The sized paper of ASA paper false proof coating has apparent hydrophobic, strain sensitivity, naked eyes i.e. distinguishable apparent
Color change, have good anti-counterfeiting performance.
Embodiment 2
（1）By the HAuCl of 55 parts by weight4With the M of 1 parts by weightwIt is dissolved in water respectively for the PVP-DADMAN of 68kg/mol, obtains dense
Degree is 1 × 10-2The HAuCl of M4Solution and a concentration of 5 × 10-6The solution of the PVP-DADMAN of M boils 1h after mixing, then add
Enter the ascorbic acid of 70 parts by weight, 98 DEG C are protected from light and are stirred to react 1h, after 10000rpm centrifuges 15min supernatant, supernatant
TEM pictures it is as shown in Figure 1；Modified Nano gold particle, average grain diameter 40nm are obtained after supernatant is dried in vacuo；
（2）By the M of 2 parts by weightwIt is dissolved in the ASA of 12 parts by weight for the PEOS of 1kg/mol, as oil phase；By step（1）It prepares
Modified Nano gold take 2 parts by weight to be dispersed in water, be made mass percentage concentration be 0.8% solution, be added dropwise dilute hydrochloric acid adjust pH
To 2, as water phase；Water phase is added in oil phase, the volume ratio of oil phase and water phase is 1:2, at room temperature ultrasonic wave stir 15min,
The Pickering lotions of oil-in-water type ASA are obtained after standing 5 days, i.e. ASA paper false proofs coating, displaing micro picture is as shown in Figure 2：
The average grain diameter of sizing agent emulsion is 2 μm, and lotion placement is unchanged for 24 hours, has good stability.
The sized paper anti-counterfeiting performance of ASA paper false proof coating is tested：
Hydrophobic anti-counterfeiting performance：The paper of test first carries out top sizing by ASA paper false proofs coating, and sizing agent dosage is 8 ‰, is applied
Glue paper surface is in light blue, and top sizing degree is 1227 seconds, with 159 ° of water contact angle, belongs to super hydrophobic surface, is had hydrophobic
Property.
Strain induction anti-counterfeiting performance：Induction is stretched, sized paper is placed on transparent glass surface, paper is clamped with pliers
And slowly pulled, the color change of sized paper is observed with light microscope, with the stretching of paper, film color is from light
Blue gradually becomes pale pink, lavender, eventually becomes red；Mechanical force impact induction, by sized paper, sizing is face-up simultaneously
Level is sprawled, and the iron block of 200g weights is taken to be suspended from above sized paper, carries out free-falling and fall to apply according to different height
On gummed paper, changing for the sized paper color after being impacted by iron block is observed and recorded with light microscope, as iron block falls
Height gradually rises, and is showed blue, pale pink and red respectively by the shock point position of the sized paper of iron block impact
Variation tendency；Perforation induction, punches sized paper with paper puncher（Circular hole）, bore hole observes hole, applies
Gummed paper perforated edge will present out different colors, be apart from the color change of hole edge from the distant to the near：Blue, pale blue
Color, pink colour, lavender and red.
The sized paper of ASA paper false proof coating has apparent hydrophobic, strain sensitivity, naked eyes i.e. distinguishable apparent
Color change, have good anti-counterfeiting performance.
Embodiment 3
（1）By the HAuCl of 20 parts by weight4With the M of 1 parts by weightwIt is dissolved in water respectively for the PVP-DADMAN of 68kg/mol, obtains dense
Degree is 1 × 10-2The HAuCl of M4Solution and a concentration of 5 × 10-6The solution of the PVP-DADMAN of M boils 1h after mixing, then add
Enter the ascorbic acid of 100 parts by weight, 98 DEG C are protected from light and are stirred to react 1h, after 20000rpm centrifuges 25min supernatant；By supernatant
Modified Nano gold particle, average grain diameter 18nm are obtained after liquid vacuum drying；
（2）By the M of 5 parts by weightwIt is dissolved in the ASA of 100 parts by weight for the PEOS of 1kg/mol, as oil phase；By step（1）System
Standby modified Nano gold takes 1 parts by weight to be dispersed in water, and the solution that mass percentage concentration is 1.2% is made, and dilute hydrochloric acid is added dropwise and adjusts
PH to 4, as water phase；Water phase is added in oil phase, the volume ratio of oil phase and water phase is 1:1, ultrasonic wave stirring at room temperature
15min obtains the Pickering lotions of oil-in-water type ASA, i.e. ASA paper false proofs coating after standing 4 days, sizing agent emulsion
Average grain diameter is 3 μm, and lotion placement is unchanged for 24 hours, has good stability.
The sized paper anti-counterfeiting performance of ASA paper false proof coating is tested：
Hydrophobic anti-counterfeiting performance：The paper of test first carries out top sizing by ASA paper false proofs coating, and sizing agent dosage is 8 ‰, is applied
Glue paper surface is in light blue, and top sizing degree is 1379 seconds, with 163 ° of water contact angle, belongs to super hydrophobic surface.
Strain induction anti-counterfeiting performance：Induction is stretched, sized paper is placed on transparent glass surface, paper is clamped with pliers
And slowly pulled, with the naked eye or the color change of optical microphotograph sem observation sized paper, with the stretching of paper, film face
Color gradually becomes pale pink, eventually becomes red from light blue；Mechanical impact force incudes, and by sized paper, sizing is face-up simultaneously
Level is sprawled, and the iron block of 1 kilogram weight is taken to be suspended from above sized paper, carries out free-falling and fall to apply according to different height
On gummed paper, changing for the sized paper color after being impacted by iron block is observed and recorded with light microscope, as iron block falls
Height gradually rises, and is showed light blue, pale pink and red respectively by the shock point position of the sized paper of iron block impact
Variation tendency；Perforation induction, punches sized paper with paper puncher（Circular hole）, bore hole observes hole,
Sized paper perforated edge will present out different colors, be apart from the color change of hole edge from the distant to the near：Blue, pale blue
Color, pale pink and red；Sized paper through ASA paper false proof coating has apparent hydrophobic, strain sensitivity, is visually
Distinguishable color change has good anti-counterfeiting performance.
Claims (8)
1. a kind of preparation method of stress induction type paper false proof coating, which is characterized in that include the following steps：
（1）By HAuCl4It is boiled after being dissolved in water with PVP-DADMAN, reducing agent is then added, be protected from light and be stirred to react, supernatant after centrifugation
Modified Nano gold particle is obtained after liquid vacuum drying；
（2）PEOS is diluted in ASA, as oil phase；By step（1）The modified Nano gold of preparation is soluble in water, adjusts pH and is
Acidity, as water phase；By water phase and oil phase, ultrasonic wave stirs in a heated condition, obtains oil-in-water type ASA's after standing
Pickering lotions, i.e. stress induction type paper false proof coating.
2. preparation method according to claim 1, which is characterized in that the weight average molecular weight M of the PVP-DADMANwFor 55-
68kg/mol；A concentration of the 1 × 10 of the PVP-DADMAN-7-1×10-5M；The HAuCl4With the mass ratio of PVP-DADMAN
It is 60:1-20:1；The HAuCl4A concentration of 1 × 10-2-1×10-4M。
3. preparation method according to claim 1, which is characterized in that the reducing agent is selected from ascorbic acid or thiocarbamide；It is excellent
It is selected as ascorbic acid；The HAuCl4Mass ratio with reducing agent is 3:1-1:5.
4. preparation method according to claim 1, which is characterized in that step（1）In, the shape of the modified Nano gold particle
Shape is nearly hexagon；Average grain diameter is 15-65nm, preferably 30-45nm.
5. preparation method according to claim 1, which is characterized in that the weight average molecular weight M of the PEOSwFor 1-3kg/
mol；The mass ratio of the PEOS and ASA is 1:3-1:10；The mass ratio of the PEOS and modified Nano gold is 1:2-5:1；
The mass percentage concentration of the modified Nano gold solution is 0.4%-1.2%.
6. preparation method according to claim 1, which is characterized in that step（2）In, the pH is 1-4；The oil phase and
The volume ratio of water phase is 1:5-1:1.
7. preparation method according to claim 1, which is characterized in that step（1）In, the boiling time is 1h；Reduction
The temperature of reaction is 98 DEG C, reaction time 1h；Centrifugal speed is 5000-20000rpm, centrifugation time 5-30min；Step
（2）In, heating temperature is 65 DEG C -80 DEG C；The time of repose is 2-5 days.
8. a kind of paper using stress induction type paper false proof coating preparation as described in claim 1.
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| CN106694039A (en) * | 2016-09-19 | 2017-05-24 | 安徽师范大学 | Preparation method and application of carbon sphere/Au nanometer composite material |
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2018
- 2018-04-25 CN CN201810378753.4A patent/CN108660852B/en active Active
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1442260A (en) * | 2002-03-01 | 2003-09-17 | 中国科学院理化技术研究所 | Preparation method of metallic nano powder |
| CN102268839A (en) * | 2011-07-25 | 2011-12-07 | 华南理工大学 | Method for preparing Pickering emulsion type alkenyl succinic anhydrides (ASA) papermaking sizing agent |
| CN105056830A (en) * | 2015-07-16 | 2015-11-18 | 齐鲁工业大学 | Biodegradable solid particle emulsifier and papermaking sizing agent |
| CN106694039A (en) * | 2016-09-19 | 2017-05-24 | 安徽师范大学 | Preparation method and application of carbon sphere/Au nanometer composite material |
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|---|---|
| CN108660852B (en) | 2020-06-30 |
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