CN111073434A - Preparation method of chromium-free fingerprint-resistant liquid - Google Patents

Preparation method of chromium-free fingerprint-resistant liquid Download PDF

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Publication number
CN111073434A
CN111073434A CN201811218368.XA CN201811218368A CN111073434A CN 111073434 A CN111073434 A CN 111073434A CN 201811218368 A CN201811218368 A CN 201811218368A CN 111073434 A CN111073434 A CN 111073434A
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China
Prior art keywords
emulsion
silicon
solution
epoxy acrylate
chromium
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CN201811218368.XA
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Chinese (zh)
Inventor
佟国峰
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Cangzhou Huarun Chemical Co ltd
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Cangzhou Huarun Chemical Co ltd
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Priority to CN201811218368.XA priority Critical patent/CN111073434A/en
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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
    • C09D151/00—Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers
    • C09D151/08—Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers grafted on to macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • 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
    • C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
    • C08F283/10—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polymers containing more than one epoxy radical per molecule

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Paints Or Removers (AREA)

Abstract

The invention relates to the technical field of metal surface treatment, in particular to a preparation method of a chromium-free fingerprint-resistant liquid, which can achieve the aim of fingerprint prevention and is harmless to human bodies and the environment; the method comprises the following steps: (1) preparing silicon-containing waterborne epoxy acrylate emulsion; (2) mixing the solvents: adding a modifier and an auxiliary crosslinking agent, and then adding 0.5-2% of EFKA3570 flatting agent according to the mass proportion of the silicon-containing water-based epoxy acrylate emulsion for high-speed dispersion; (3) diluting silicon-containing waterborne epoxy acrylate emulsion; (4) dispersing at high speed; (5) and (4) placing.

Description

Preparation method of chromium-free fingerprint-resistant liquid
Technical Field
The invention relates to the technical field of metal surface treatment, in particular to a preparation method of a chromium-free fingerprint-resistant liquid.
Background
In recent years, along with the improvement of living standard of people, the popularity of electronic products such as televisions, computers and mobile phones is higher and higher, the appearance requirements of people on the objects are higher and higher, but in the using process of the electronic products, fingerprints of users can be attached to the surface of a metal product, the attractiveness of the products is influenced, the phenomenon that the parts attached with the fingerprints are easy to rust and corrode is easy to occur, the product performance is influenced finally, the service life of the products is shortened, and the problem is solved by the invention of a fingerprint-resistant treatment technology which is characterized in that the fingerprint-resistant treatment is realized by Cr3+And Cr6+A compact chromate conversion film with a self-healing function and strong corrosion resistance is generated on a part to be treated to achieve the fingerprint resistance effect, but hexavalent chromium elements with high toxicity and high carcinogenicity are contained in the conversion film to cause harm to human bodies and the environment, so that the market urgently needs to research a chromium-free fingerprint-resistant liquid. Not only can achieve the purpose of preventing fingerprints, but also is harmless to human bodies and the environment.
The color difference meter is widely applied to the field of color management of industries such as plastic, printing, paint ink, textile, printing and dyeing clothes, measures and displays a color difference △ E value of a sample and a measured sample according to Lab and Lch principles of CIE color space, is suitable for color evaluation and data control inside and outside an enterprise, and △ E ═ △ L ═ 2+ (△ a) 2+ (△ b)2]1/2 , △ L = L sample-L standard (lightness difference), △ a = a sample-a standard (red/green difference), △ b = b sample-b standard (yellow/blue difference), the template △ E after being processed by the fingerprint-resistant processing technique was 0.2, and the smaller △ E was, the more excellent.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method of a chromium-free fingerprint-resistant liquid which can achieve the aim of fingerprint prevention and is harmless to human bodies and the environment.
The preparation method of the chromium-free fingerprint-resistant liquid comprises the following steps:
(1) preparation of silicon-containing waterborne epoxy acrylate emulsion: emulsion polymerization is one of free radical polymerization modes, monomers are subjected to free radical polymerization in a water phase by means of an emulsifier, the monomers are emulsified into uniform and stable emulsion, and acrylic acid, organic silicon and epoxy resin are copolymerized to synthesize silicon-containing waterborne epoxy acrylate emulsion with stable performance;
(2) mixing the solvents: adding a modifier and an auxiliary crosslinking agent, and then adding 0.5-2% of EFKA3570 flatting agent according to the mass proportion of the silicon-containing water-based epoxy acrylate emulsion for high-speed dispersion;
(3) diluting the silicon-containing water-based epoxy acrylate emulsion: slowly adding deionized water in the dispersing process, and diluting the content of the emulsion to 10-30%;
(4) high-speed dispersion: continuously dispersing for 10-30 minutes after the deionized water is added;
(5) placing: pouring the dispersed emulsion into a container for later use.
The preparation method of the chromium-free fingerprint-resistant liquid comprises the following steps of:
a. adding alkylphenol polyoxyethylene and lauryl sodium sulfate into a calculated amount of deionized water, heating to dissolve, and adding sodium bicarbonate to completely dissolve to obtain a solution A;
b. dissolving an initiator acrylonitrile-styrene-butadiene copolymer in water to obtain a solution B;
c. mixing an acrylic monomer, epoxy resin and an organic silicon monomer to obtain a mixed solid A; adding 0.5 of the solution A and 0.1 of the mixed solid A into a four-neck flask, stirring at room temperature for 10min at the rotating speed of 300-500 r/min to obtain a solution C;
d. adding the 0.5 solution B into the four-neck flask, heating to 80 ℃, keeping the temperature constant after reaching 80 ℃, and keeping the temperature for 0.5 hour;
e. after the heat preservation is finished, adding the residual solution A and the mixed solid A, and adding a certain amount of residual solution B at intervals in the adding process;
f. after the addition is finished, heating to 85 ℃, and preserving heat for 1.5 hours after the temperature is reached;
g. after the heat preservation is finished, slowly cooling to 30 ℃, adjusting the pH value of the emulsion to be between 7 and 8 by using ammonia water, and then filtering by using a 100-mesh sieve to obtain the silicon-containing waterborne epoxy acrylate emulsion.
According to the preparation method of the chromium-free fingerprint-resistant liquid, the modifier used in the step (2) is preferably one or more of aminosilane, alkylsilane and phenylsilane.
According to the preparation method of the chromium-free fingerprint-resistant liquid, 0.7-1.4% of EFKA3570 flatting agent is preferably added in the step (2).
According to the preparation method of the chromium-free fingerprint-resistant liquid, 1% of EFKA3570 flatting agent is preferably added in the step (2).
According to the preparation method of the chromium-free fingerprint-resistant liquid, the dispersion is preferably continued for 20 minutes after the deionized water is added in the step (4).
Compared with the prior art, the invention has the beneficial effects that: the invention relates to alkylphenol polyoxyethylene, lauryl sodium sulfate, sodium bicarbonate, acrylic acid monomer and epoxy resinGrease, organic silicon monomer, ammonia water, amino silane, alkyl silane, phenyl silane, an auxiliary crosslinking agent and EFKA3570 deionized water do not contain chromium elements, a color difference meter is widely applied to the color management field of the industries such as plastics, printing, paint ink, textile, printing and dyeing clothes, the color difference meter is used for measuring and displaying the color difference △ E value of a sample and a measured sample according to the Lab and Lch principles of CIE color space, and is suitable for internal and external color evaluation and data management and control, wherein △ E ═ 2 [ (△ L) 2+ (△ a) 2+ (△ b)2]1/2 , △ L = L sample-L standard (lightness difference), △ a = a sample-a standard (red/green difference), △ b = b sample-b standard (yellow/blue difference), a sample plate △ E after being processed by the fingerprint resistant processing technology is 0.2, and △ E is more excellent as the size is smaller, the △ E value of the chromium-free fingerprint resistant liquid prepared by the method is less than 0.2, and therefore the purposes of fingerprint resistance and no harm to human bodies and the environment are achieved.
Detailed Description
The following examples are given to further illustrate the embodiments of the present invention. The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
Example 1
Adding alkylphenol polyoxyethylene and lauryl sodium sulfate into a calculated amount of deionized water, heating to dissolve, and adding sodium bicarbonate to completely dissolve to obtain a solution A; dissolving an initiator acrylonitrile-styrene-butadiene copolymer in water to obtain a solution B; mixing an acrylic monomer, epoxy resin and an organic silicon monomer to obtain a mixed solid A; adding 0.5 of the solution A and 0.1 of the mixed solid A into a four-neck flask, stirring at room temperature for 10min at the rotating speed of 300-500 r/min to obtain a solution C; adding the 0.5 solution B into the four-neck flask, heating to 80 ℃, keeping the temperature constant after reaching 80 ℃, and keeping the temperature for 0.5 hour; after the heat preservation is finished, adding the residual solution A and the mixed solid A, and adding a certain amount of residual solution B at intervals in the adding process; after the addition is finished, heating to 85 ℃, and preserving heat for 1.5 hours after the temperature is reached; after the heat preservation is finished, slowly cooling to 30 ℃, adjusting the pH value of the emulsion to be between 7 and 8 by using ammonia water, and then filtering by using a 100-mesh sieve to obtain the silicon-containing waterborne epoxy acrylate emulsion.
Adding one or more of aminosilane, alkyl silane and phenyl silane and an auxiliary crosslinking agent, then adding 1% of EFKA3570 flatting agent according to the mass proportion of the silicon-containing waterborne epoxy acrylate emulsion, carrying out high-speed dispersion, slowly adding deionized water in the dispersion process, diluting the emulsion to 15%, continuing to disperse for 20 minutes after the deionized water is completely added, and pouring the dispersed emulsion into a container for later use.
Example 2
Adding alkylphenol polyoxyethylene and lauryl sodium sulfate into a calculated amount of deionized water, heating to dissolve, and adding sodium bicarbonate to completely dissolve to obtain a solution A; dissolving an initiator acrylonitrile-styrene-butadiene copolymer in water to obtain a solution B; mixing an acrylic monomer, epoxy resin and an organic silicon monomer to obtain a mixed solid A; adding 0.5 of the solution A and 0.1 of the mixed solid A into a four-neck flask, stirring at room temperature for 10min at the rotating speed of 300-500 r/min to obtain a solution C; adding the 0.5 solution B into the four-neck flask, heating to 80 ℃, keeping the temperature constant after reaching 80 ℃, and keeping the temperature for 0.5 hour; after the heat preservation is finished, adding the residual solution A and the mixed solid A, and adding a certain amount of residual solution B at intervals in the adding process; after the addition is finished, heating to 85 ℃, and preserving heat for 1.5 hours after the temperature is reached; after the heat preservation is finished, slowly cooling to 30 ℃, adjusting the pH value of the emulsion to be between 7 and 8 by using ammonia water, and then filtering by using a 100-mesh sieve to obtain the silicon-containing waterborne epoxy acrylate emulsion.
Adding one or more of aminosilane, alkyl silane and phenyl silane and an auxiliary crosslinking agent, then adding 1% of EFKA3570 flatting agent according to the mass proportion of the silicon-containing waterborne epoxy acrylate emulsion, carrying out high-speed dispersion, slowly adding deionized water in the dispersion process, diluting the emulsion to 30%, continuing to disperse for 20 minutes after the deionized water is completely added, and pouring the dispersed emulsion into a container for later use.
Example 3
Adding alkylphenol polyoxyethylene and lauryl sodium sulfate into a calculated amount of deionized water, heating to dissolve, and adding sodium bicarbonate to completely dissolve to obtain a solution A; dissolving an initiator acrylonitrile-styrene-butadiene copolymer in water to obtain a solution B; mixing an acrylic monomer, epoxy resin and an organic silicon monomer to obtain a mixed solid A; adding 0.5 of the solution A and 0.1 of the mixed solid A into a four-neck flask, stirring at room temperature for 10min at the rotating speed of 300-500 r/min to obtain a solution C; adding the 0.5 solution B into the four-neck flask, heating to 80 ℃, keeping the temperature constant after reaching 80 ℃, and keeping the temperature for 0.5 hour; after the heat preservation is finished, adding the residual solution A and the mixed solid A, and adding a certain amount of residual solution B at intervals in the adding process; after the addition is finished, heating to 85 ℃, and preserving heat for 1.5 hours after the temperature is reached; after the heat preservation is finished, slowly cooling to 30 ℃, adjusting the pH value of the emulsion to be between 7 and 8 by using ammonia water, and then filtering by using a 100-mesh sieve to obtain the silicon-containing waterborne epoxy acrylate emulsion.
Adding one or more of aminosilane, alkyl silane and phenyl silane and an auxiliary crosslinking agent, then adding 1% of EFKA3570 flatting agent according to the mass proportion of the silicon-containing waterborne epoxy acrylate emulsion, carrying out high-speed dispersion, slowly adding deionized water in the dispersion process, diluting the emulsion content to 20%, continuing to disperse for 20 minutes after the deionized water is completely added, and pouring the dispersed emulsion into a container for later use.
The emulsion prepared in the above example was applied to a member to be treated, and then the color difference value △ E of the member to be treated was measured by a color difference meter, and the following results were obtained:
example 1 Example 2 Example 3
△E 0.18 0.13 0.17
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.

Claims (6)

1. The preparation method of the chromium-free fingerprint-resistant liquid is characterized by comprising the following steps:
(1) preparation of silicon-containing waterborne epoxy acrylate emulsion: emulsion polymerization is one of free radical polymerization modes, monomers are subjected to free radical polymerization in a water phase by means of an emulsifier, the monomers are emulsified into uniform and stable emulsion, and acrylic acid, organic silicon and epoxy resin are copolymerized to synthesize silicon-containing waterborne epoxy acrylate emulsion with stable performance;
(2) mixing the solvents: adding a modifier and an auxiliary crosslinking agent, and then adding 0.5-2% of EFKA3570 flatting agent according to the mass proportion of the silicon-containing water-based epoxy acrylate emulsion for high-speed dispersion;
(3) diluting the silicon-containing water-based epoxy acrylate emulsion: slowly adding deionized water in the dispersing process, and diluting the content of the emulsion to 10-30%;
(4) high-speed dispersion: and continuing to disperse for 10-30 minutes after the deionized water is added.
(5) Placing: pouring the dispersed emulsion into a container for later use.
2. The method for preparing a chromium-free fingerprint-resistant liquid as claimed in claim 1, wherein the preparation of the silicon-containing aqueous epoxy acrylate emulsion in the step (1) comprises the steps of:
a. adding alkylphenol polyoxyethylene and lauryl sodium sulfate into a calculated amount of deionized water, heating to dissolve, and adding sodium bicarbonate to completely dissolve to obtain a solution A;
b. dissolving an initiator acrylonitrile-styrene-butadiene copolymer in water to obtain a solution B;
c. mixing an acrylic monomer, epoxy resin and an organic silicon monomer to obtain a mixed solid A; adding 0.5 of the solution A and 0.1 of the mixed solid A into a four-neck flask, stirring at room temperature for 10min at the rotating speed of 300-500 r/min to obtain a solution C;
d. adding the 0.5 solution B into the four-neck flask, heating to 80 ℃, keeping the temperature constant after reaching 80 ℃, and keeping the temperature for 0.5 hour;
e. after the heat preservation is finished, adding the residual solution A and the mixed solid A, and adding a certain amount of residual solution B at intervals in the adding process;
f. after the addition is finished, heating to 85 ℃, and preserving heat for 1.5 hours after the temperature is reached;
g. after the heat preservation is finished, slowly cooling to 30 ℃, adjusting the pH value of the emulsion to be between 7 and 8 by using ammonia water, and then filtering by using a 100-mesh sieve to obtain the silicon-containing waterborne epoxy acrylate emulsion.
3. The method for preparing a chromium-free fingerprint resistant liquid as claimed in claim 1, wherein the modifier used in the step (2) is one or more of aminosilane, alkylsilane and phenylsilane.
4. The method for preparing a chrome-free fingerprint resistant liquid as claimed in claim 1, wherein preferably, 0.7% to 1.4% EFKA3570 leveling agent is added in the step (2).
5. The method for preparing a chrome-free fingerprint resistant liquid as claimed in claim 1, wherein preferably 1% EFKA3570 leveling agent is added in the step (2).
6. The method for preparing a chromium-free fingerprint-resistant liquid as claimed in claim 1, wherein the dispersion is continued for 20 minutes after the deionized water is added in the step (4).
CN201811218368.XA 2018-10-19 2018-10-19 Preparation method of chromium-free fingerprint-resistant liquid Pending CN111073434A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103555156A (en) * 2013-09-27 2014-02-05 上海维凯化学品有限公司 Ultraviolet-curable anti-fingerprint antistatic paint composition
KR101444701B1 (en) * 2013-04-10 2014-09-26 건설화학공업 주식회사 Ultraviolet curable coating composition for polyvinylchloride flooring with the excellent anti-fingerprint

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101444701B1 (en) * 2013-04-10 2014-09-26 건설화학공업 주식회사 Ultraviolet curable coating composition for polyvinylchloride flooring with the excellent anti-fingerprint
CN103555156A (en) * 2013-09-27 2014-02-05 上海维凯化学品有限公司 Ultraviolet-curable anti-fingerprint antistatic paint composition

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
胡娟: ""无铬耐指纹剂的制备、表征及应用"", 《万方数据知识服务平台》 *
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Application publication date: 20200428