CN104356839A - Anti-light-ageing reinforcement material of colored relics and preparation method of reinforcement material - Google Patents
Anti-light-ageing reinforcement material of colored relics and preparation method of reinforcement material Download PDFInfo
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- CN104356839A CN104356839A CN201410566015.4A CN201410566015A CN104356839A CN 104356839 A CN104356839 A CN 104356839A CN 201410566015 A CN201410566015 A CN 201410566015A CN 104356839 A CN104356839 A CN 104356839A
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- reinforcement material
- colored drawing
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- historical relic
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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
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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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/20—Diluents or solvents
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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
- 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
- C09D7/61—Additives non-macromolecular inorganic
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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
- 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
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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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/65—Additives macromolecular
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
Abstract
The invention discloses an anti-light-ageing reinforcement material of colored relics. The reinforcement material is prepared from the following components in parts by weight: 500-1,200 parts of silicon dioxide, 6,000-20,000 parts of B72, 5-40 parts of polyethylene glycol octylphenol ether, 4-20 parts of aminopropyl triethoxy silane, 5,000-80,000 parts of a 85%-95% ethanol aqueous solution and 30,000-200,000 parts of ethyl acetate. Compared with a common reinforcement material B72 of the colored relics, the anti-light-ageing reinforcement material is relatively long in service life and relatively high in stability, especially, the light ageing resistance is remarkably improved, and a preparation process of the anti-light-ageing reinforcement material is simple and convenient to perform.
Description
Technical field
The present invention relates to a kind of colored drawing historical relic anti-light aging reinforcement material and preparation method thereof, belong to Techniques of Relics Protection field.
Background technology
Colored drawing historical relic refers on the matrix such as ceramic, Shi Zhi, apply to be mixed with sizing material pigment and the historical relic made.Have a very wide distribution in China, to there is quantity many, famous The Terra Cotta Warriors and Horses of Qin colored drawing pottery, Dunhuang frescoes are Typical Representatives of colored drawing historical relic.Colored drawing historical relic has high historical value, artistic value and scientific value, but the sizing material under optical radiation in colored drawing historical relic can occur aging, pigment is come off, and wherein many colored drawing historical relics are in Critical Condition, have become the plain pottery figurine of grey as The Terra Cotta Warriors and Horses of Qin colored drawing pottery.Conventional guard method utilizes reinforcement material to carry out conservation treatment to improve the stability of color, and the colored drawing historical relic reinforcement material generally used at present is B72(acrylic resin).But along with deepening continuously of historical relic's protection work, the poor shortcoming of B72 light fastness aging reveals gradually.Under optical radiation, B72 molecular chain is degraded, and occurs the fissions such as jaundice becomes fragile, intensity step-down, have impact on the effect of colored drawing historical relic's protection.
Summary of the invention
An object of the present invention is to provide that a kind of life-span is long, stability is high, the reinforcement material of anti-light aging ability significant anti-colored drawing historical relic photoaging.
Another object of the present invention is to the preparation method that above-mentioned historical relic reinforcement material is provided.
For achieving the above object, the technical solution used in the present invention is:
A kind of colored drawing historical relic anti-light aging reinforcement material, prepared by following component, each component and weight part thereof are:
Silicon-dioxide 500 ~ 1200
B72 6000～20000
Triton X-100 5 ~ 40
Aminopropyl triethoxysilane 4 ~ 20
85 ~ 95% aqueous ethanolic solutions 5000 ~ 80000
Ethyl acetate 30000 ~ 200000.
Preferred component and weight part thereof are:
Silicon-dioxide 750 ~ 1100
B72 9300～16000
Triton X-100 5 ~ 30
Aminopropyl triethoxysilane 4 ~ 10
85 ~ 95% aqueous ethanolic solutions 5000 ~ 50000
Ethyl acetate 30000 ~ 100000.
Described silicon-dioxide is nano silicon, and its particle diameter is 5 ~ 100nm.
The preparation method of above-mentioned colored drawing historical relic anti-light aging reinforcement material, comprises the following steps:
(1) preparation of solution A
Triton X-100, aminopropyl triethoxysilane and silicon-dioxide are added in 85 ~ 95% aqueous ethanolic solutions;
(2) preparation of solution B
B72 is dissolved in ethyl acetate;
(3) solution A uniformly emulsify (preferably adopting ultrasonic wave dispersion) is mixed to obtain solution C with solution B afterwards, obtain colored drawing historical relic anti-light aging reinforcement material.
In above-mentioned materials, add Triton X-100 (OP-10) and aminopropyl triethoxysilane (KH550) is to reduce SiO
2reunion.
The reinforcement material of the above-mentioned anti-colored drawing historical relic photoaging prepared, for being slightly albescent liquid, adopts brushing or spraying method to carry out conservation treatment to colored drawing historical relic.In order to improve protected effect, process again after evaporation of the solvent, suggestion consolidation process 2 ~ 3 times next time.Increase ethyl acetate consumption, rarer proportioning can be obtained, only need repeatedly spray treatment can reach same provide protection.
Reinforcement material of the present invention is longer than the life-span of conventional colored drawing historical relic reinforcement material B72, stability is higher, and particularly anti-light aging ability significantly increases.Its preparation technology is simple, easy to operate.
Accompanying drawing explanation
Fig. 1 is the infrared spectra curve before and after aging 240 hours of B72 film, 1-a be aging before; 1-b be aging after;
Fig. 2 is the infrared spectra curve before and after aging 240 hours of material membrane of the present invention, 2-a be aging before; 2-b be aging after;
Fig. 3 be ester group characteristic peak in photo aging process absorbance A reduce per-cent (wave number is about 1170cm
-1 ), 3-a is B72 film; 3-b is material membrane of the present invention.
Embodiment
Below in conjunction with embodiment, the present invention will be further described, so that the more detailed advantage setting forth the inventive method.
Testing mould material used is utilize solution C direct formation of film at surface after naturally volatilizing, and film thickness is 0.3 ~ 0.5mm about; Colored drawing sample block is brushing gelatin and mineral color malachite green on ceramic base plate, and surface is again through the material reinforced process of anti-light aging of the present invention.B72 main component used is 1:2 methyl acrylate and ethyl methacrylate copolymers.
Embodiment 1
(1) anti-light aging reinforcement material preparation
Take 1.25g Nano-meter SiO_2
2add the dehydrated alcohol/deionized water mixed solvent 100mL of volume ratio 85/15, add 0.0125g KH550 and 0.0375g OP-10 obtain solution A.Take 2g B72, be dissolved in obtain solution B in 8g ethyl acetate.
At 60 DEG C, by solution A ultrasonic disperse 120min.Getting above-mentioned solution A 12.8mL after ultrasonic disperse adds in 10g solution B, namely obtains SiO of the present invention
2-B72 compound anti-colored drawing historical relic photoaging reinforcement material.Above-mentioned reinforcement material is evenly painted on film forming on slide glass, brushes and repeat brushing once after the surface seasoning of colored drawing sample block, the sample ambient temperatare after process is put after 1 week and is used;
(2) anti-light aging Performance Detection
The mould material of preparation and colored drawing sample block are placed in apart from UVA ultraviolet source 2cm place (average UV light irradiance 180 μ W/cm
2) irradiation, by detecting the FTIR spectrum characteristic of each sample in weathering process, mechanical strength, hydrophobic nature, the change of color and rate of weight loss etc. with the anti-light aging performance of test material.
Test the infrared spectra, weight and the wetting angle to water that utilize Tensor 27 Fourier infrared spectrograph, BP211D-OCE type precision balance and JJ-1 type Wetness Angle Measuring Instrument measurement mould material respectively, coordinate the fixture (utility model patent: ZL 2,010 2 0110534.7) of self-developing development to measure the mechanical strength of thin-film material with PT-1176 universal testing machine, utilize SP65 type portable colorimeter to measure the colour-change of colored drawing sample block.
1) change of mould material infrared spectra in photo aging process
Fig. 1 and Fig. 2 is respectively the infrared spectra curve of B72 film and material membrane of the present invention aging 240 hours front and back, can find out that the infrared spectra change of material membrane of the present invention is little compared with B72 film.In weathering process, 1170cm
-1near wave number, the absorbance A reduction per-cent of ester group characteristic peak is shown in Fig. 3, illustrates in identical digestion time, and the absorbancy of the characteristic peak of material of the present invention reduces per-cent and is less than B72.When being aged to 240h, the absorbancy of this characteristic peak of B72 decreases beyond 90%, and material absorbancy of the present invention reduces only 50%.As can be seen here, material molecule structural modification of the present invention is less, and its anti-light aging performance significantly improves.
2) weightlessness of mould material in photo aging process
In photo aging process, the rate of weight loss of sample is Wp, and its calculation formula is:
Wp = [(Wa-Wb)/Wa] ×100%
In formula: Wa-aging front sample quality;
Wb-aged samples quality;
After 276h is aging, material rate of weight loss of the present invention is only 8%, B72 rate of weight loss about 10%, illustrates that material anti-light aging performance of the present invention increases.
3) change of mould material mechanical property in photo aging process
After optical radiation, the increase of B72 fragility, intensity reduce, and easily produce fragmentation, fracture, directly have influence on the protected effect of colored drawing historical relic after External Force Acting.Material of the present invention adds inorganic nano material in B72 matrix, the balancing effect of the stress concentration of nanoparticle and stress radiation is utilized to make polymkeric substance without obvious stress concentration phenomenon, utilize transmission ofenergy effect to make polymkeric substance crackle diffusion hindered and passivation and reduce destructive cracking, the mechanical property improving polymeric matrix makes its activeness and quietness.
Experiment adopts universal testing machine to coordinate self-made clamp to test, sensor 5Kg, probe translational speed 100mm/min.First sample thin film is fixed on fixture circular hole during test, probe in the mobile material-testing machine be positioned at directly over it is to film surface and punctured, record the maximum, force F(kg born when film punctures), and calculate corresponding intensity σ (MPa), its calculation formula is formula:
σ=[(3/2)FS]÷BH
2
Wherein, H is film thickness (mm), B, and to be film width (mm), S be measures the span (mm) of fulcrum.
Photoaging
4after 32h, the detected result of the mechanical property of each mould material is in table 1, and wherein B and S is 2mm, and sample number into spectrum B0 and B1 is respectively B72 and material of the present invention.Experimental result illustrates that the mechanical property of material of the present invention obtains obvious improvement, and its intensity is about 3 times of B72.
4) change of mould material hydrophobicity performance in photo aging process
Organic polymer material has certain hydrophobic nature, but in use along with aging its hydrophobic nature of continuous generation reduces gradually.Experimental result shows, aging through 108h, and B72 contact angle reduces and is greater than 50%, and reduce only 25% through material angle of the present invention, the hydrophobicity performance of material of the present invention is well kept in weathering process, and anti-light aging performance is significantly improved.
5) colour-change of colored drawing sample block in photo aging process
At present, the aberration systematic quantification represented the change of material color usual L a b in the world describes, Δ E(value of chromatism) represent the change of material color, the change of the larger material color of its value is more obvious.The mathematic(al) representation of Δ E is as follows:
ΔE= [(ΔL)
2 + (Δa)
2 + (Δb)
2]
1/2
Wherein: a is red green product coordinates, and b is champac chromaticity coordinate, and L is brightness.
After 432h is aging, the colour-change of colored drawing sample block is in table 2, and the colour-change Δ E of visible contrast colored drawing sample block (the colored drawing sample block through B72 process) is 2.59, and the colour-change Δ E of the colored drawing sample block of material processing of the present invention is 1.08; And colour-change mainly comes from the increase of Δ b, and namely sample there occurs xanthochromia.Illustrate under photoirradiation, B72 aging yellowing easier in the present invention material, and anti-light aging reinforcement material of the present invention significantly improve than the anti-light aging performance of conventional historical relic's protection material B 72.Time like this to colored drawing historical relic's protection, be conducive to the historical relic's protection principle following " not changing historical relic original appearance ", this is the most basic principle of colored drawing historical relic's protection.
Embodiment 2
Preparation method is similar with embodiment 1, can prepare the water-proof material described in table 3.
Embodiment 3
Similar with embodiment 1, change SiO in solution by the add-on changing solution A and solution B
2concentration, experimental results is in table 4.
From table 4, material of the present invention comparatively B72 anti-light aging performance is significantly improved, the anti-light aging improved performance degree of material of the present invention and SiO
2concentration is relevant, and SiO
2concentration is higher, and effect is better.
Claims (5)
1. a colored drawing historical relic anti-light aging reinforcement material, is prepared by following component, and each component and weight part thereof are:
Silicon-dioxide 500 ~ 1200
B72 6000～20000
Triton X-100 5 ~ 40
Aminopropyl triethoxysilane 4 ~ 20
85 ~ 95% aqueous ethanolic solutions 5000 ~ 80000
Ethyl acetate 30000 ~ 200000.
2. colored drawing historical relic anti-light aging reinforcement material according to claim 1, is characterized in that each component and weight part thereof are:
Silicon-dioxide 750 ~ 1100
B72 9300～16000
Triton X-100 5 ~ 30
Aminopropyl triethoxysilane 4 ~ 10
85 ~ 95% aqueous ethanolic solutions 5000 ~ 50000
Ethyl acetate 30000 ~ 100000.
3. colored drawing historical relic anti-light aging reinforcement material according to claim 1, it is characterized in that: described silicon-dioxide is nano silicon, its particle diameter is 5 ~ 100nm.
4. the preparation method of colored drawing historical relic anti-light aging reinforcement material described in claim 1, is characterized in that comprising the following steps:
(1) preparation of solution A
Triton X-100, aminopropyl triethoxysilane and silicon-dioxide are added in 85 ~ 95% aqueous ethanolic solutions;
(2) preparation of solution B
B72 is dissolved in ethyl acetate;
(3) mix to obtain solution C by after solution A uniformly emulsify with solution B, obtain colored drawing historical relic anti-light aging reinforcement material.
5. the preparation method of colored drawing historical relic anti-light aging reinforcement material according to claim 4, is characterized in that: in step (3), and the emulsification of solution A adopts ultrasonic wave dispersion.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410566015.4A CN104356839A (en) | 2014-10-23 | 2014-10-23 | Anti-light-ageing reinforcement material of colored relics and preparation method of reinforcement material |
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|---|---|---|---|
| CN201410566015.4A CN104356839A (en) | 2014-10-23 | 2014-10-23 | Anti-light-ageing reinforcement material of colored relics and preparation method of reinforcement material |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108085011A (en) * | 2017-12-19 | 2018-05-29 | 山东鸿扬文物保护工程有限公司 | A kind of semi-moist or humid region earthen ruins strengthening agent and reinforcement means |
| CN110079178A (en) * | 2019-03-08 | 2019-08-02 | 上海大学 | It the protectant preparation method of transparent hydrophobic and its is applied in historical relic's protection |
| CN112210238A (en) * | 2020-10-13 | 2021-01-12 | 广东潮鑫建设工程有限公司 | Cultural relic protection repair complementary color matching method |
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| CN103992729A (en) * | 2014-05-07 | 2014-08-20 | 陕西师范大学 | Reinforcing agent for crisp powder ceramic painted cultural relic |
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| CN103360889A (en) * | 2013-07-31 | 2013-10-23 | 陕西师范大学 | Stone colored drawing reinforcing agent |
| CN103992729A (en) * | 2014-05-07 | 2014-08-20 | 陕西师范大学 | Reinforcing agent for crisp powder ceramic painted cultural relic |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108085011A (en) * | 2017-12-19 | 2018-05-29 | 山东鸿扬文物保护工程有限公司 | A kind of semi-moist or humid region earthen ruins strengthening agent and reinforcement means |
| CN108085011B (en) * | 2017-12-19 | 2021-02-26 | 山东鸿扬文物保护工程有限公司 | Reinforcing agent and reinforcing method for earthen site in semi-moist or moist area |
| CN110079178A (en) * | 2019-03-08 | 2019-08-02 | 上海大学 | It the protectant preparation method of transparent hydrophobic and its is applied in historical relic's protection |
| CN112210238A (en) * | 2020-10-13 | 2021-01-12 | 广东潮鑫建设工程有限公司 | Cultural relic protection repair complementary color matching method |
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Application publication date: 20150218 |