CN112175439B - Nano ferric oxide ultraviolet-proof additive and preparation method thereof - Google Patents

Nano ferric oxide ultraviolet-proof additive and preparation method thereof Download PDF

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CN112175439B
CN112175439B CN202010878478.XA CN202010878478A CN112175439B CN 112175439 B CN112175439 B CN 112175439B CN 202010878478 A CN202010878478 A CN 202010878478A CN 112175439 B CN112175439 B CN 112175439B
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CN112175439A (en
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梁峰
郭玲娟
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Zhejiang Zhengqi Shirong Technology Co ltd
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    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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    • C09D7/61—Additives non-macromolecular inorganic
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    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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    • C09D7/65—Additives macromolecular
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Abstract

The application relates to the field of nano iron oxide, and particularly discloses a nano iron oxide ultraviolet-proof additive and a preparation method thereof. The nanometer ferric oxide ultraviolet-proof additive is prepared from the following raw materials in parts by weight: 40-60 parts of nano iron oxide, 10-15 parts of a dispersing agent, 20-30 parts of an effervescent agent and 8-10 parts of an accelerating agent. The preparation method comprises the following steps: s1: pretreating the nano iron oxide by using a dispersing agent; s2: mechanically stirring and mixing the pretreated nano iron oxide, the accelerant and the effervescent agent; s3: the mixture stirred in step S2 was tabletted. The nano iron oxide ultraviolet-proof additive has the advantage of providing better ultraviolet resistance; in addition, the preparation method has the advantage of improving the dispersion uniformity of all components of the ultraviolet-proof additive.

Description

Nano ferric oxide ultraviolet-proof additive and preparation method thereof
Technical Field
The application relates to the field of nano iron oxide, in particular to a nano iron oxide ultraviolet-proof additive and a preparation method thereof.
Background
When the polymer material is used outdoors, the polymer material is degraded due to the irradiation of sunlight and the like, so that the appearance of a polymer product is deteriorated, and the physical and mechanical properties are reduced. However, the ultraviolet absorber can suppress such a photo-aging effect, thereby extending the service life of the polymer material.
The nano iron oxide has the characteristics of nano particles, such as surface effect, small-size effect, quantum size effect and the like, and the currently applied iron oxide is mainly alpha-Fe2O3. Nano alpha-Fe2O3Has excellent magnetism, higher catalytic activity, good light resistance, weather resistance and ultraviolet ray shielding capability, and is widely applied to ultraviolet filters and various paint ultraviolet ray-proof additives.
In view of the above-mentioned related technologies, the nano iron oxide has a strong surface effect due to the characteristics of its nano particles, and when it is added into a formulation of a coating material or the like for mixing, it is easy to agglomerate due to the surface effect of the nano particles immediately after the addition, and the agglomerated nano iron oxide has a significantly reduced ultraviolet resistance for the coating material due to the increased particle size.
Disclosure of Invention
In order to weaken the agglomeration effect when the nano iron oxide is added, the application provides the nano iron oxide ultraviolet-proof additive and the preparation method thereof.
In a first aspect, the application provides a nano iron oxide ultraviolet-proof additive, which adopts the following technical scheme:
the nanometer ferric oxide ultraviolet-proof additive is prepared from the following raw materials in parts by weight: 40-60 parts of nano iron oxide, 10-15 parts of a dispersing agent, 20-30 parts of an effervescent agent and 8-10 parts of an accelerating agent.
By adopting the technical scheme, the nano iron oxide has better ultraviolet shielding capability and can play a main role in ultraviolet resistance, but the nano iron oxide has strong surface effect due to the small size of particles, has very high surface area, is easy to agglomerate when being added into various solvents and loses the ultraviolet resistance of the nano iron oxide. Under the action of the dispersing agent, the nano iron oxide can be well dispersed and is not easy to agglomerate. The addition of the accelerator further improves the ultraviolet resistance of the ultraviolet-proof additive. The addition of effervescent agent makes ultraviolet protection additive when adding the use, effervescent agent can produce a large amount of bubbles in the solvent, the bubble of production, the mechanical stirring effect that the bubble formed at the cracked in-process of come-up can carry out more profitable dispersion effect to each component including nanometer iron oxide in the additive, avoid the reunion effect of nanometer iron oxide on the one hand, on the other hand makes each component of additive can disperse fast, not extremely high condition to the even degree requirement of dispersion, can not even need the manual work to carry out mechanical stirring, it is higher to improve the efficiency of the dispersed ground of material.
And the effervescent agent and the nano iron oxide are synchronously put into use, so that at the beginning of the putting, the effervescent agent can generate bubbles to avoid the agglomeration action when the nano iron oxide is just mixed, and further avoid the agglomeration phenomenon of the nano iron oxide to the maximum extent.
Preferably, the dispersant comprises the following components in percentage by weight: 10-30% of sodium dodecyl benzene sulfonate, 10-30% of polyepoxysuccinic acid and the balance of polyethylene glycol.
By adopting the technical scheme, the sodium dodecyl benzene sulfonate and the polyepoxysuccinic acid are both anionic surfactants, and the electrostatic force and the spatial repulsive force of a nano material system are changed due to the adsorption of the negatively charged groups on the surface of the nano material, so that the stability of the nano iron oxide in the solvent is improved, and the nano iron oxide is not easy to agglomerate. Researches show that the polyethylene glycol has a modification effect on the nano iron oxide and has a dispersing and stabilizing effect on the nano iron oxide, so that the nano iron oxide particles have a better dispersing effect.
Preferably, the effervescent agent comprises the following components in percentage by weight: 20-30% of an alkaline agent, 20-30% of an acid agent, 10-20% of polyvinylpyrrolidone dissolved in ethanol and the balance dextrin.
By adopting the technical scheme, after the alkali agent and the acid agent meet water, carbonate particles in the alkali agent and hydrogen ions in the acid agent are ionized to be separated from constraint, and react to generate a large amount of carbon dioxide gas bubbles, so that the effects of effervescence, stirring and dispersion are achieved. The components in the effervescent agent, which is dissolved in ethanol and water and is used as an adhesive, are bonded with other components in the ultraviolet-proof additive, and the finally obtained ultraviolet-proof additive cannot be formed. When the ethanol water solution of the polyvinylpyrrolidone and the polyepoxysuccinic acid in the dispersant coexist, a synergistic effect can be generated, the dispersion effect of the polyvinylpyrrolidone and the polyepoxysuccinic acid in the additive system is greatly improved, and the stability of the dispersed nano iron oxide system is also greatly improved.
Preferably, the alkaline agent is selected from one or more of sodium bicarbonate, potassium bicarbonate and sodium carbonate.
By adopting the technical scheme, the sodium bicarbonate, the potassium bicarbonate and the sodium carbonate are solid at normal temperature, contain more carbonate ions and can release more bubbles, thereby achieving a better effervescent effect.
Preferably, the acid agent is selected from one or more of acetic acid, tartaric acid, citric acid.
By adopting the technical scheme, because the acetic acid, the tartaric acid and the citric acid have low acid strength, the acetic acid, the tartaric acid and the citric acid are selected as the main components of the acid agent, so that the acid agent can not generate strong acidity under the condition of providing hydrogen ions, and has great influence on the acid-base environment after the addition of the additive.
Preferably, the accelerator comprises the following components in percentage by weight: 20-40% of benzotriazole, 10-30% of benzophenone, 10-20% of triazine and the balance of acetone.
By adopting the technical scheme, hydrogen bonds are formed among carbonyl oxygen and hydroxyl hydrogen of the benzophenone and between N and H in triazine and benzotriazole, and after ultraviolet irradiation, the hydrogen bonds can be oscillated and opened to absorb ultraviolet rays and release the ultraviolet rays in a heat energy mode, so that the function of absorbing the ultraviolet rays is achieved. The acetone is used as a solvent, and the components with ultraviolet absorption capacity of the three components are dissolved and dispersed uniformly, so that the accelerator is dispersed uniformly in the final product as a whole.
Preferably, 10-20 parts of bentonite is further added into the nano iron oxide ultraviolet-proof additive.
By adopting the technical scheme, the bentonite has stronger adsorption performance, can gather molecular adsorption to the surface of the bentonite, the bentonite is firstly mixed with the accelerant, the accelerant is adsorbed to the surface of the bentonite, and then the bentonite is dispersed by the disintegration and foaming effects of the effervescent agent when in use, so that the proportion of each component of the accelerant is basically uniform, and meanwhile, the whole accelerant component is uniformly dispersed in the solution along with the bentonite. The surface of the bentonite generally has negative charges and can adsorb cations, and in the disintegration process of an acid agent and an alkali agent in the effervescent agent, the cations are adsorbed by the bentonite, so that the effervescent effect is better, more and faster bubbles are generated, and the mechanical stirring effect is better.
In a second aspect, the application provides a preparation method of a nano iron oxide ultraviolet-proof additive, which adopts the following technical scheme:
a preparation method of a nano ferric oxide ultraviolet-proof additive comprises the following steps:
s1: pretreating the nano iron oxide by using a dispersing agent to obtain pretreated nano iron oxide;
s2: mixing and stirring the accelerant and the bentonite uniformly to obtain a pre-stirred mixture;
s3: mechanically stirring and mixing the pretreated nano iron oxide, the pre-stirred mixture and the effervescent agent to obtain a mixture;
s4: and (5) drying and tabletting the mixture stirred in the step S2 to obtain the nano iron oxide ultraviolet-proof additive.
By adopting the technical scheme, the dispersant is firstly mixed with the nano iron oxide for pretreatment, and the dispersant can be firstly attached to the nano iron oxide, so that the dispersing capacity of the nano iron oxide is improved in advance. And then mixing the accelerant and bentonite, and uniformly adsorbing the accelerant components by the bentonite through adsorption, so that the ultraviolet-proof additive formed by mixing the pretreated nano iron oxide, the pre-stirred mixture and the effervescent agent has better gradation and uniformity.
In summary, the present application has the following beneficial effects:
1. because the application adopts a compounding mode of mixing the dispersing agent, the accelerating agent, the effervescing agent and the nano-iron oxide, the effect of reducing the agglomeration of the nano-iron oxide is obtained due to the chemical dispersing effect of the dispersing agent and the instant foaming of the effervescing agent.
2. In the application, the polyepoxysuccinic acid is preferably used as a component of the dispersing agent, and the ethanol water solution of the polyvinylpyrrolidone is preferably used as the adhesive, so that the synergistic dispersing effect is achieved between the polyepoxysuccinic acid and the polyvinylpyrrolidone, and the effect of optimizing the dispersion stability of the nano iron oxide is obtained.
3. According to the method, the components are orderly and uniformly combined through step-by-step treatment, and finally, the product is obtained through pressing, so that a better dispersion uniformity effect is obtained.
Detailed Description
The present application will be described in further detail with reference to examples.
Examples
Example 1
The nanometer ferric oxide ultraviolet-proof additive is prepared from the following raw materials in parts by weight: 40 parts of nano iron oxide, 10 parts of a dispersing agent, 20 parts of an effervescent agent and 8 parts of an accelerating agent.
The dispersant comprises the following components in percentage by weight: 10% of ethylene diamine tetraacetic acid, 10% of polyepoxysuccinic acid and 80% of polyethylene glycol.
The effervescent agent comprises the following components in percentage by weight: 20% of an alkaline agent, 20% of an acid agent, 10% of polyvinylpyrrolidone dissolved in ethanol and 50% of dextrin.
The alkaline agent is selected from sodium bicarbonate.
The acid agent is selected from acetic acid.
In the ethanol-water solution of the polyvinylpyrrolidone, the mass fraction of the polyvinylpyrrolidone is 5%, and the volume fraction of the ethanol in the ethanol-water solution is 75%.
The accelerant comprises the following components in percentage by weight: 20% of benzotriazole, 30% of benzophenone, 20% of triazine and 30% of acetone. The triazine is cyanuric acid.
The preparation method of the nano ferric oxide ultraviolet-proof additive specifically comprises the following steps:
s1: pretreating nano-iron oxide, stirring and uniformly mixing ethylene diamine tetraacetic acid, polyepoxysuccinic acid and polyethylene glycol according to a proportion to obtain a dispersant mixed solution, then spraying the dispersant mixed solution to the surface of the nano-iron oxide through an atomizing gun, and after spraying is finished, collecting the dispersant mixed solution dripping from the nano-iron oxide and continuously spraying the dispersant mixed solution to the surface of the nano-iron oxide until no dispersant mixed solution drips.
S2: mixing the raw materials; the method comprises the steps of stirring, dissolving and uniformly mixing acetone, benzophenone, cyanuric acid and benzotriazole according to a proportion to obtain an accelerator liquid mixture, and then evaporating acetone and drying at 50 ℃ by using an oven to obtain an accelerator solid mixture. And then mechanically stirring and granulating the pretreated solid mixture of the nano iron oxide, the effervescent agent and the accelerant.
S3: and (5) tabletting, namely tabletting the final raw material mixture obtained in the step S2 by using a tabletting machine to obtain a finished product of the nano ferric oxide ultraviolet-proof additive.
The differences between examples 2 to 5 and example 1 are shown in the following table:
Figure BDA0002653360760000071
Figure BDA0002653360760000081
example 6
The nanometer ferric oxide ultraviolet-proof additive is prepared from the following raw materials in parts by weight: 60 parts of nano iron oxide, 15 parts of a dispersing agent, 30 parts of an effervescent agent, 10 parts of an accelerating agent and 10 parts of bentonite.
The dispersant comprises the following components in percentage by weight: 30% of ethylene diamine tetraacetic acid, 30% of polyepoxysuccinic acid and 40% of polyethylene glycol.
The effervescent agent comprises the following components in percentage by weight: 30% of an alkaline agent, 30% of an acid agent, 20% of polyvinylpyrrolidone dissolved in ethanol and 20% of dextrin.
The alkaline agent is selected from sodium bicarbonate.
The acid agent is selected from acetic acid.
The accelerant comprises the following components in percentage by weight: 20% of benzotriazole, 10% of benzophenone, 20% of triazine and 50% of acetone. The triazine is cyanuric acid.
The preparation method of the nano ferric oxide ultraviolet-proof additive specifically comprises the following steps:
s1: pretreating nano-iron oxide, stirring and uniformly mixing ethylene diamine tetraacetic acid, polyepoxysuccinic acid and polyethylene glycol according to a proportion to obtain a dispersant mixed solution, then spraying the dispersant mixed solution to the surface of the nano-iron oxide through an atomizing gun, and after spraying is finished, collecting the dispersant mixed solution dripping from the nano-iron oxide and continuously spraying the dispersant mixed solution to the surface of the nano-iron oxide until no dispersant mixed solution drips.
S2: mixing the raw materials; and stirring, dissolving and uniformly mixing the acetone, the benzophenone, the cyanuric acid and the benzotriazole according to a ratio to obtain an accelerator liquid mixture, then adding the bentonite into the accelerator liquid mixture according to a ratio, and uniformly stirring to obtain a secondary mixture. The acetone in the second mixture was then evaporated in an oven at 50 ℃ and dried to give a solid mixture of the promoter. And then mechanically stirring and granulating the pretreated solid mixture of the nano iron oxide, the effervescent agent and the accelerant.
S3: and (5) tabletting, namely tabletting the final raw material mixture obtained in the step S2 by using a tabletting machine to obtain a finished product of the nano iron oxide ultraviolet-proof additive.
Example 7 differs from example 6 in that: the addition amount of bentonite is 15 parts by weight.
Example 8 differs from example 6 in that: the addition amount of bentonite is 20 parts by weight.
Example 9 differs from example 1 in that: the alkaline agent is a mixture of sodium bicarbonate and sodium carbonate with the mass ratio of 1: 1; the acid agent is a mixture of acetic acid and tartaric acid with a mass ratio of 1: 1.
Example 10 differs from example 1 in that: the agent is a mixture of sodium bicarbonate, sodium carbonate and potassium bicarbonate with the mass ratio of 1: 1; the acid agent is selected from acetic acid, tartaric acid and citric acid at a mass ratio of 1: 1.
Comparative example
Comparative example 1
The ultraviolet-proof additive is pure nano iron oxide.
Comparative example 2
The difference from example 1 is that: the raw materials of the ultraviolet-proof additive are not added with an effervescent agent.
Comparative example 3
The difference from example 1 is that: the raw materials of the ultraviolet-proof additive are not added with a dispersant.
Comparative example 4
The difference from example 1 is that: polyepoxysuccinic acid in the dispersant component is replaced by equivalent amount of ethylene diamine tetraacetic acid.
Performance test
A3 steel with specification of 15mm 10mm 2mm is selected. Grinding with sand paper to 1000#, polishing, removing oil with acetone, ultrasonic cleaning, and blow-drying with hair dryer.
The coating is polyurethane varnish of Tianjin lighthouse GmbH, diluted by acetone when in use, and the mass ratio of the varnish to the solvent is 1: 4.
The UV blocking additives of examples 1 to 10 and comparative examples 1 to 4 were added to the varnish solution, then A3 steel was dip-coated, cured at room temperature for 24 hours, and then placed in a drying oven to be dried at 60 ℃ for 24 hours for full curing, and the thickness was measured with a micrometer thickness gauge, and the dry film thickness was about 30 μm.
The aging test chamber adopts a quartz lamp tube with a Bocheng 253nm light source, the temperature is 25 ℃, and the relative humidity is 70% +/-5%.
The steel after the coating curing was placed in an aging test chamber and irradiated for 14 days, and then taken out for analysis by EIS.
Porosity can be measured by the theoretical resistance (R) of the coating at which the porosity is "infinitept) And measured pore resistance (R)p) Is determined by the ratio of (a). The calculation formula is as follows: porosity ═ Rpt/Rp(RptD is the coating thickness, a is the electrode area, k is the electrolyte conductivity, 4.2Sm-1)
Rpt＝30×10-6/(150×10-6×4.2)＝0.048Ω
TABLE 1
Examples Rp(Ω×104) P
Example 1 113 4.25×10-8
Example 2 112 4.29×10-8
Example 3 111 4.32×10-8
Example 4 113 4.25×10-88
Example 5 112 4.29×10-8
Example 6 118 4.07×10-8
Example 7 116 4.14×10-8
Example 8 116 4.14×10-8
Example 9 117 4.10×10-8
Example 10 119 4.03×10-8
Comparative example 1 24 2.00×10-7
Comparative example 2 47 1.02×10-7
Comparative example 3 45 1.07×10-7
Comparative example 4 86 5.58×10-8
As can be seen by combining examples 1-10 and comparative examples 1-4 and combining Table 1, the porosity of examples 1-10 is less than that of comparative examples 1-4, which indicates that the UV resistant additive used in the present application is more uniformly dispersed in the coating and has better optimization for the UV resistance of the coating. The comparison of the results of the comparative example 1 and the example 1 shows that under the same conditions, the ultraviolet resistance of the ultraviolet-proof additive adopted in the application is obviously superior to that of the additive which is only added with the nano iron oxide, while the comparison of the results of the comparative examples 2 and 3 and the example 1 shows that the effervescent agent and the dispersing agent play a better role in dispersing and anti-agglomeration of the nano iron oxide, and the ultraviolet resistance of the nano iron oxide in the coating to the coating is obviously improved. Finally, as can be seen by comparing the comparative example 4 with the example 1, the polyepoxysuccinic acid and the polyvinylpyrrolidone have a certain synergistic effect, and the dispersing effect of the dispersant after the polyepoxysuccinic acid is adopted on the nano iron oxide is obviously improved.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.

Claims (5)

1. The nano iron oxide ultraviolet-proof additive is characterized by being prepared from the following raw materials in parts by weight: 40-60 parts of nano iron oxide, 10-15 parts of a dispersing agent, 20-30 parts of an effervescent agent and 8-10 parts of an accelerating agent;
the dispersant comprises the following components in percentage by weight: 10-30% of ethylene diamine tetraacetic acid, 10-30% of polyepoxysuccinic acid and the balance of polyethylene glycol;
the effervescent agent comprises the following components in percentage by weight: 20-30% of an alkaline agent, 20-30% of an acid agent, 10-20% of polyvinylpyrrolidone dissolved in ethanol and the balance of dextrin;
the accelerant comprises the following components in percentage by weight: 20-40% of benzotriazole, 10-30% of benzophenone, 10-20% of triazine and the balance of acetone.
2. The nano iron oxide ultraviolet protection additive of claim 1, wherein: the alkaline agent is selected from one or more of sodium bicarbonate, potassium bicarbonate and sodium carbonate.
3. The nano iron oxide ultraviolet protection additive of claim 1, wherein: the acid agent is selected from one or more of acetic acid, tartaric acid and citric acid.
4. The nano iron oxide ultraviolet protection additive of claim 1, wherein: 10-20 parts of bentonite is further added into the nano iron oxide ultraviolet-proof additive.
5. The method for preparing the nano iron oxide ultraviolet ray prevention additive as recited in any one of claims 1 to 4, wherein: the method comprises the following steps:
s1: pretreating the nano iron oxide by using a dispersing agent to obtain pretreated nano iron oxide;
s2: mechanically stirring and mixing the pretreated nano iron oxide, the accelerant and the effervescent agent to obtain a mixture;
s3: and (4) tabletting the mixture stirred in the step S2 to obtain the nano iron oxide ultraviolet-proof additive.
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EP3315575A1 (en) * 2015-06-26 2018-05-02 M. Technique Co., Ltd. Method for producing ultraviolet protective agent composition, and ultraviolet protective agent composition obtained thereby

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EP3315575A1 (en) * 2015-06-26 2018-05-02 M. Technique Co., Ltd. Method for producing ultraviolet protective agent composition, and ultraviolet protective agent composition obtained thereby
CN105001718A (en) * 2015-07-24 2015-10-28 吴江市屯村颜料厂 Pigment red 112 dispersions and preparation method thereof

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