CN108467650A - A kind of preparation method of hydrophilic antifogging material - Google Patents
A kind of preparation method of hydrophilic antifogging material Download PDFInfo
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- CN108467650A CN108467650A CN201810247992.6A CN201810247992A CN108467650A CN 108467650 A CN108467650 A CN 108467650A CN 201810247992 A CN201810247992 A CN 201810247992A CN 108467650 A CN108467650 A CN 108467650A
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- container
- hydrophilic
- initiator
- added dropwise
- coating
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- 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
- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
- C09D133/24—Homopolymers or copolymers of amides or imides
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/58—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide containing oxygen in addition to the carbonamido oxygen, e.g. N-methylolacrylamide, N-(meth)acryloylmorpholine
-
- 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/63—Additives non-macromolecular organic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/58—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide containing oxygen in addition to the carbonamido oxygen, e.g. N-methylolacrylamide, N-(meth)acryloylmorpholine
- C08F220/585—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide containing oxygen in addition to the carbonamido oxygen, e.g. N-methylolacrylamide, N-(meth)acryloylmorpholine and containing other heteroatoms, e.g. 2-acrylamido-2-methylpropane sulfonic acid [AMPS]
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Materials Applied To Surfaces To Minimize Adherence Of Mist Or Water (AREA)
- Paints Or Removers (AREA)
Abstract
It is antifog to achieve the effect that since common anti-fog coating is to add surfactant in a manner of physical bond in hydrophilic coating on the market, it is lost the disadvantage is that surfactant is easy dissolving in water, coating is made to lose anti misting capability.In order to solve the problems, such as this, the present invention proposes a kind of preparation method of hydrophilic antifogging coating liquid, hydrophilic antifogging coating liquid structure based on acrylic acid copolymer, introduce a large amount of amide groups and hydroxyl or other hydrophilic radicals, the hardness and hydrophilic effect of coating is respectively increased, response type nonionic surfactant is accessed using chemical bond simultaneously, makes coating that there is more preferable hydrophily, more longlasting anti-fog effect and water resistance.
Description
Technical field
The present invention relates to water wetted material field technologies, are specifically related to a kind of preparation method of hydrophilic antifogging material.
Background technology
Currently, the common anti-fog coating in market is usually to add surface-active in a manner of physical bond in hydrophilic coating
Agent, it is antifog to achieve the effect that, it is lost the disadvantage is that surfactant is easy dissolving in water, coating is made to lose anti misting capability.
Invention content
In view of this, in order to solve problem above, the present invention proposes a kind of preparation method of hydrophilic antifogging material, this is hydrophilic
Anti misting materials structure based on acrylic acid copolymer introduces a large amount of amide groups and hydroxyl or other hydrophilic radicals, carries respectively
The hardness and hydrophilic effect of high coating, while response type nonionic surfactant is accessed using chemical bond, so that coating is had more
Good hydrophily, more longlasting anti-fog effect and water resistance.
A kind of preparation method of hydrophilic antifogging material comprising following steps：
S1 opens the electric mixer of container one, and in the state that stirrer is kept stirring, and it is 5 to sequentially add mass ratio：4：
Then 3 alcohol, alcohol ether and deionized water adds the response type nonionic surfactant of certain mass, wherein response type is non-
Ionic surface active agent accounts for the 0.6% of the gross mass of the above alcohol, alcohol ether and deionized water, is followed by stirring for heating up, and the dynamics of stirring is
Liquid level is kept to eddy, temperature is set as 80 DEG C, heating-up time 30min；
S2, by acrylic acid, acrylate, acrylic amide function monomer, alcohol and deionized water according to mass ratio be 3.5：3：5：
2：8 ratio is added to successively in container two, and is mixed, and monomer mixture solution is configured to；
S3, by alcohol and water according to mass ratio be 7：3 ratio mixing is added in container three, and azodiisobutyronitrile initiation is added
Agent, hereinafter referred to as AIBN, form initiator mixed liquor, and wherein AIBN accounts for the gross mass of finally formed initiator mixed liquor
0.8%；Wherein, the response type nonionic surfactant in container one account for container one in step S1, in step S2 container two and step
The 0.3% of the quality of all raw materials in rapid S3 in container three, the acrylic amide function monomer in container two, which accounts in step S1, to be held
The 3.53% of the quality of all raw materials in device one, step S2 in container two and step S3 in container three, the initiator in container three
Account for container one in step S1, the quality of all raw materials in step S2 in container two and step S3 in container three 0.75%；
The initiator solution of 2/3 amount of the monomer mixed solution in container two in container three is respectively charged into and is dripped into constant pressure by S4
In liquid funnel, and at the uniform velocity it is added dropwise into container one simultaneously, time for adding is 2~3 hours, and rate of addition control was dripped at 2 seconds one,
The temperature of reaction is controlled at 80 ± 1 DEG C；
The initiator of remaining 1/3 amount in container three is encased in constant pressure funnel by S5, reaction mixing in step s 4
After liquid keeps the temperature half an hour, the initiator of remaining 1/3 amount to be divided 2 times and is added dropwise, the interval time being added dropwise twice is 30min,
Rate of addition is about to drip for 0.5 second one, and control is added dropwise every time and is added dropwise in 10min, 80 DEG C of reaction temperature, after being added dropwise
Heat preservation 3 hours, finally stirring are cooled to 30 DEG C, keep 30min that can take the dish out of the pot；
A concentration of 10%NaOH solution is added in the synthetic resin into step S5 in container three so that the synthesis in step S5 in S6
Resin becomes neutral；
S7, by 6：2：2：1.5：It is solid that 0.1 mass ratio weighs synthetic resin, alcoholic solvent, amino resins in step S6 successively
Agent, water and alkylsulfonate stir evenly, you can to obtain the preparation method of the hydrophilic antifogging coating liquid of the present invention.
Further, the acrylic amide function monomer packet in a kind of preparation method of hydrophilic antifogging material as described above
Include one in hydroxymethyl acrylamide, hydroxypropylacrylamide, Diacetone Acrylamide, 2- acrylamide-2-methyl propane sulfonics
Kind is a variety of.
As shown in Figure 1, the reaction principle of the preparation method for the hydrophilic antifogging coating liquid of the present invention, hydroxymethyl acrylamide
Or other acrylamide monomers and acrylic acid copolymer, the CH on right side2CHCCL-R is the response type nonionic based on propenyl chloride
Surfactant participates in combined polymerization and forms segment, by adding amino resins or Blocked Isocyanate Curing Agents and part hydroxyl
Base and carboxyl react to form reticular structure, remaining-groups such as OH ,-COOH ,-R provide hydrophilic antifogging effect, amide group
Introducing effectively strengthens coating hardness.
Description of the drawings
It is the reaction principle of the preparation method for the hydrophilic antifogging material that the present invention is the present invention as shown in Figure 1.
Following specific implementation mode will be further illustrated the present invention in conjunction with above-mentioned attached drawing.
Specific implementation mode
A kind of preparation method of hydrophilic antifogging material comprising following steps：
S1 opens the electric mixer of container one, and in the state that stirrer is kept stirring, and it is 5 to sequentially add mass ratio：4：
Then 3 alcohol, alcohol ether and deionized water adds the response type nonionic surfactant of certain mass, wherein response type is non-
Ionic surface active agent accounts for the 0.6% of the gross mass of the above alcohol, alcohol ether and deionized water, is followed by stirring for heating up, and the dynamics of stirring is
Liquid level is kept to eddy, temperature is set as 80 DEG C, heating-up time 30min；
S2, by acrylic acid, acrylate, acrylic amide function monomer, alcohol and deionized water according to mass ratio be 3.5：3：5：
2：8 ratio is added to successively in container two, and is mixed, and monomer mixture solution is configured to；
S3, by alcohol and water according to mass ratio be 7：3 ratio mixing is added in container three, and azodiisobutyronitrile initiation is added
Agent, hereinafter referred to as AIBN, form initiator mixed liquor, and wherein AIBN accounts for the gross mass of finally formed initiator mixed liquor
0.8%；Wherein, the response type nonionic surfactant in container one account for container one in step S1, in step S2 container two and step
The 0.3% of the quality of all raw materials in rapid S3 in container three, the acrylic amide function monomer in container two, which accounts in step S1, to be held
The 3.53% of the quality of all raw materials in device one, step S2 in container two and step S3 in container three, the initiator in container three
Account for container one in step S1, the quality of all raw materials in step S2 in container two and step S3 in container three 0.75%；
The initiator solution of 2/3 amount of the monomer mixed solution in container two in container three is respectively charged into and is dripped into constant pressure by S4
In liquid funnel, and at the uniform velocity it is added dropwise into container one simultaneously, time for adding is 2~3 hours, and rate of addition control was dripped at 2 seconds one,
The temperature of reaction is controlled at 80 ± 1 DEG C；
The initiator of remaining 1/3 amount in container three is encased in constant pressure funnel by S5, reaction mixing in step s 4
After liquid keeps the temperature half an hour, the initiator of remaining 1/3 amount to be divided 2 times and is added dropwise, the interval time being added dropwise twice is 30min,
Rate of addition is about to drip for 0.5 second one, and control is added dropwise every time and is added dropwise in 10min, 80 DEG C of reaction temperature, after being added dropwise
Heat preservation 3 hours, finally stirring are cooled to 30 DEG C, keep 30min that can take the dish out of the pot；
A concentration of 10%NaOH solution is added in the synthetic resin into step S5 in container three so that the synthesis in step S5 in S6
Resin becomes neutral；
S7, by 6：2：2：1.5：It is solid that 0.1 mass ratio weighs synthetic resin, alcoholic solvent, amino resins in step S6 successively
Agent, water and alkylsulfonate stir evenly, you can to obtain the preparation method of the hydrophilic antifogging coating liquid of the present invention.
The above hydrophilic antifogging material is stirred evenly, is then coated on clean resin substrate, is toasted with 130 DEG C
30min forms a film, and is then tested, test result is as follows：
| Detection project | Detection method | Examination criteria | Result judgement |
| Appearance of coat | Range estimation | Water white transparency, the coating surfaces defect such as no blistering, crackle, orange peel | It is qualified |
| Light transmittance | Ultra-violet and visible spectrophotometer | ≥95% | 98% |
| It is antifog | It is stifling above 80 DEG C of water surface 5cm | It does not haze within 10 minutes | It is qualified |
| Hardness | Pencil hardometer | With reference to GB/T 6739-2006, the pencil hardness of film is measured using QHQ-A type pencil hardometers | 3H |
| It is water-fast | It is impregnated for 24 hours in water | With reference to GB/T 1733-1993, film is soaked in deionized water, sees whether bubble, white, off phenomenon | It is qualified |
| Adhesive force | Hundred lattice are tested | With reference to GB/T 9286-1998, the adhesive force of film is measured by the method for drawing lattice experiment using HGQ types paint film lattice drawing device | 1 grade or more |
As shown in Figure 1, for the present invention hydrophilic antifogging material preparation method reaction principle, hydroxymethyl acrylamide or other
Acrylamide monomer and acrylic acid copolymer, the CH on right side2CHCCL-R is that the response type non-ionic surface based on propenyl chloride is lived
Property agent, participate in combined polymerization and form segment, pass through and add amino resins or Blocked Isocyanate Curing Agents and part of hydroxyl and carboxylic
Base reacts to form reticular structure, remaining-groups such as OH ,-COOH ,-R provide hydrophilic antifogging effect, the introducing of amide group has
Effect strengthens coating hardness.
Several embodiments of the invention above described embodiment only expresses, the description thereof is more specific and detailed, but simultaneously
Cannot the limitation to the scope of the claims of the present invention therefore be interpreted as.It should be pointed out that for those of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the guarantor of the present invention
Protect range.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (2)
1. a kind of preparation method of hydrophilic antifogging material comprising following steps：
S1 opens the electric mixer of container one, and in the state that stirrer is kept stirring, and it is 5 to sequentially add mass ratio：4：
Then 3 alcohol, alcohol ether and deionized water adds the response type nonionic surfactant of certain mass, wherein response type is non-
Ionic surface active agent accounts for the 0.6% of the gross mass of the above alcohol, alcohol ether and deionized water, is followed by stirring for heating up, and the dynamics of stirring is
Liquid level is kept to eddy, temperature is set as 80 DEG C, heating-up time 30min；
S2, by acrylic acid, acrylate, acrylic amide function monomer, alcohol and deionized water according to mass ratio be 3.5：3：5：
2：8 ratio is added to successively in container two, and is mixed, and monomer mixture solution is configured to；
S3, by alcohol and water according to mass ratio be 7：3 ratio mixing is added in container three, and azodiisobutyronitrile initiation is added
Agent, hereinafter referred to as AIBN, form initiator mixed liquor, and wherein AIBN accounts for the gross mass of finally formed initiator mixed liquor
0.8%；Wherein, the response type nonionic surfactant in container one account for container one in step S1, in step S2 container two and step
The 0.3% of the quality of all raw materials in rapid S3 in container three, the acrylic amide function monomer in container two, which accounts in step S1, to be held
The 3.53% of the quality of all raw materials in device one, step S2 in container two and step S3 in container three, the initiator in container three
Account for container one in step S1, the quality of all raw materials in step S2 in container two and step S3 in container three 0.75%；
The initiator solution of 2/3 amount of the monomer mixed solution in container two in container three is respectively charged into and is dripped into constant pressure by S4
In liquid funnel, and at the uniform velocity it is added dropwise into container one simultaneously, time for adding is 2~3 hours, and rate of addition control was dripped at 2 seconds one,
The temperature of reaction is controlled at 80 ± 1 DEG C；
The initiator of remaining 1/3 amount in container three is encased in constant pressure funnel by S5, reaction mixing in step s 4
After liquid keeps the temperature half an hour, the initiator of remaining 1/3 amount to be divided 2 times and is added dropwise, the interval time being added dropwise twice is 30min,
Rate of addition is about to drip for 0.5 second one, and control is added dropwise every time and is added dropwise in 10min, 80 DEG C of reaction temperature, after being added dropwise
Heat preservation 3 hours, finally stirring are cooled to 30 DEG C, keep 30min that can take the dish out of the pot；
A concentration of 10%NaOH solution is added in the synthetic resin into step S5 in container three so that the synthesis in step S5 in S6
Resin becomes neutral；
S7, by 6：2：2：1.5：It is solid that 0.1 mass ratio weighs synthetic resin, alcoholic solvent, amino resins in step S6 successively
Agent, water and alkylsulfonate stir evenly, you can to obtain target product anti-fog coating.
2. the preparation method of hydrophilic antifogging material as described in claim 1, it is characterised in that：It is as described above a kind of hydrophilic anti-
Acrylic amide function monomer in the preparation method of mist material includes hydroxymethyl acrylamide, hydroxypropylacrylamide, double third
It is one or more in ketone acrylamide, 2- acrylamide-2-methyl propane sulfonics.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810247992.6A CN108467650A (en) | 2018-03-23 | 2018-03-23 | A kind of preparation method of hydrophilic antifogging material |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810247992.6A CN108467650A (en) | 2018-03-23 | 2018-03-23 | A kind of preparation method of hydrophilic antifogging material |
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| Publication Number | Publication Date |
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| CN108467650A true CN108467650A (en) | 2018-08-31 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201810247992.6A Pending CN108467650A (en) | 2018-03-23 | 2018-03-23 | A kind of preparation method of hydrophilic antifogging material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109439094A (en) * | 2018-09-12 | 2019-03-08 | 安徽康瑞高科新材料技术工程有限公司 | A kind of method that hydrocolloid particle prepares pollution resistance hydrophilic coating |
| CN110078859A (en) * | 2019-05-30 | 2019-08-02 | 江苏中新瑞光学材料有限公司 | The preparation process of the super hydrophilic material of optical grade |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102850924A (en) * | 2012-09-21 | 2013-01-02 | 中国海洋石油总公司 | Antifogging coating long in antifogging life |
-
2018
- 2018-03-23 CN CN201810247992.6A patent/CN108467650A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102850924A (en) * | 2012-09-21 | 2013-01-02 | 中国海洋石油总公司 | Antifogging coating long in antifogging life |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109439094A (en) * | 2018-09-12 | 2019-03-08 | 安徽康瑞高科新材料技术工程有限公司 | A kind of method that hydrocolloid particle prepares pollution resistance hydrophilic coating |
| CN110078859A (en) * | 2019-05-30 | 2019-08-02 | 江苏中新瑞光学材料有限公司 | The preparation process of the super hydrophilic material of optical grade |
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Application publication date: 20180831 |
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