CN108084872A - A kind of decayed rock historical relic strengthening agent and preparation method thereof - Google Patents
A kind of decayed rock historical relic strengthening agent and preparation method thereof Download PDFInfo
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- CN108084872A CN108084872A CN201711248024.9A CN201711248024A CN108084872A CN 108084872 A CN108084872 A CN 108084872A CN 201711248024 A CN201711248024 A CN 201711248024A CN 108084872 A CN108084872 A CN 108084872A
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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
- C09D4/00—Coating compositions, e.g. paints, varnishes or lacquers, based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; Coating compositions, based on monomers of macromolecular compounds of groups C09D183/00 - C09D183/16
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
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Abstract
The invention belongs to historical relic reinforcement technique fields, disclose a kind of decayed rock historical relic strengthening agent and preparation method thereof.The decayed rock historical relic strengthening agent of the present invention is obtained by the component reaction for including following mass parts meter：60~98 parts of esters of silicon acis；0~30 part of organosilicon compound；1.2~12.8 parts of deionized waters；0.01~0.1 part of hydrolyst；0~6 part of diluent；0~16 part of filler；0~0.6 part of catalyst.After the present invention is contacted using the functional group of hydrolyzable present in strengthening agent with the moisture in air, hydrolysis-condensation reaction can occur rapidly, generated so as to cause strengthening agent inside and cure crosslinking, form tridimensional network.This curing agent can be effectively penetrated into the hole and crack of decayed rock, be bonded as one the rock of weathering by curing crosslinking, improved the intensity of rock historical relic.The decayed rock historical relic strengthening agent hardening time of the present invention can be adjusted according to construction requirement, solidification effect significantly improves.
Description
Technical field
The invention belongs to historical relic reinforcement technique field, more particularly to a kind of decayed rock historical relic strengthening agent and its preparation side
Method.
Background technology
In the protection work of historical relic, the protection of rock historical relic is very important problem.Exposure in the wild numerous big
Type stone matter historic site, including building, rock cave, stone tablet, city wall, house etc., due to the slacking and human factor of natural cause
Destroy, many cultural artifact surfaces have occurred and that serious degradation phenomena, decorative pattern is unclear, crisp alkali, dusting, peeling, Rockmass fractures etc..Such as
It does not adopt an effective measure, the historical relic of many preciousnesses will not exist, so developing stone cultural artifact defencive function material of good performance
Material has become one of urgent task of historical relic's protection research field.In order to which this degradation phenomena is controlled to occur, protection rock text
Object, through rock cultural artifact surface is infiltrated frequently with chemical material, spray, brush or apply etc. modes, to improve its weather resistance
Ability improves its intensity.
Research to decayed rock historical relic reinforcement material, foreign countries report it is more, be broadly divided into organic strengthening agent and it is inorganic plus
Gu agent；Organic strengthening agent is mostly with lotion, polyurethane, epoxy resin etc..It is verified through overaging, finds lotion in the process used
In, due to the presence of water, rock historical relic can be made to come off or even cave in；And organic strengthening agent such as polyurethane, epoxy resin is then easily old
The adverse effects such as change, poor permeability, this is not permitted in historical relic's protection.
It is well known that the main component of rock historical relic is silica.Present invention applicant prepares by substantial amounts of experiment
A kind of moisture-free has the organic silicon strengthening agent of Adjustable viscosity；The strengthening agent of low viscosity has excellent permeability,
Rock interior can be penetrated into along the hole of rock itself；High viscosity strengthening agent can be filled into crack and the hollowing of decayed rock
In, so as to which the component of decayed rock be bonded as one again, recover the intensity of rock, achieve the purpose that reinforcing.
The content of the invention
In order to overcome the shortcomings and deficiencies of the prior art described above, primary and foremost purpose of the invention is to provide a kind of decayed rock
Historical relic strengthening agent, be adjusted with viscosity, moisture-free, solidification intensity height, water-tolerant, to historical relic without destroy spy
Point.
Another object of the present invention is to provide a kind of preparation method of above-mentioned decayed rock historical relic strengthening agent.
The purpose of the present invention is realized by following proposal：
A kind of decayed rock historical relic strengthening agent is obtained by the component reaction for including following mass parts meter：
60~98 parts of esters of silicon acis；
0~30 part of organosilicon compound；
1.2~12.8 parts of deionized waters；
0.01~0.1 part of hydrolyst；
0~6 part of diluent；
0~16 part of filler；
0~0.6 part of catalyst.
The structural formula of the organosilicon compound is as follows：
R1-Si-(OR2)3Or (R1,R3)-Si-(OR2)2
Wherein R1、R3Identical or different is respectively alkyl, aryl, alkenyl, aralkyl or alkaryl；R2For methyl or
Ethyl.
In the decayed rock historical relic strengthening agent of the present invention, the esters of silicon acis may include methyl orthosilicate, silester, silicon
Propyl propionate, butyl silicate, four (1- Methylethyls) esters of silicon acis, four phenyl ester of silicic acid, four (2- ethyl-butyls) esters of silicon acis and four (2- second
At least one of base base) esters of silicon acis.
The esters of silicon acis is preferably at least one of silester Si-28, Si-32 and Si-40；More preferably silicic acid
Ethyl ester Si-40；More preferably silester Si-40 of the viscosity average molecular weigh 700~780.
In the organosilicon compound：
The alkyl may include methyl (CH3-, Me), ethyl (CH3CH2-, Et), propyl (CH3CH2CH2-, n-Pr), it is different
Propyl ((CH3)2CH-, i-Pr), normal-butyl (CH3CH2CH2CH2-, n-Bu), isobutyl group ((CH3)2CHCH2-, i-Bu), sec-butyl
(CH3CH2(CH3) CH-, s-Bu), tertiary butyl ((CH3)3C-, t-Bu) etc..
The aryl may include phenyl (C6H5-, Ph), 1- how base (C12H7-, naPh), 2- how base (C12H7-, 2-naPh)
Deng.
The alkenyl may include vinyl (CH2=CH-), pi-allyl (CH2=CH-CH2-), acrylic (CH3CH=
CH-), isopropenyl (- (CH3) C=CH2) etc..
The aralkyl may include benzyl (C6H5-CH2-), phenethyl (C6H5-CH2-CH2-) etc..
The alkaryl may include o- tolyl (CH3-C6H4-), m- tolyl (CH3-C6H4-), p- tolyl
(CH3-C6H4-), o- ethylbenzene (CH3CH2-C6H4-), m- ethylbenzene (CH3CH2-C6H4-), p- ethylbenzene (CH3CH2-
C6H4-) etc..
Aqueous hydrochloric acid solution, aqueous sulfuric acid, aqueous solution of nitric acid, phosphate aqueous solution, first can be selected in the hydrolyst
Acid and acetic acid.
The aqueous hydrochloric acid solution, aqueous sulfuric acid, the mass percent concentration of aqueous solution of nitric acid are 2~15%；It is described
Phosphate aqueous solution mass percent concentration be 8~30%；The formic acid and the mass percent concentration of acetic acid for 60~
90%.
The diluent can be selected in methanol, ethyl alcohol, normal propyl alcohol, isopropanol, n-butanol, isobutanol, ether at least
One kind is preferably at least one of methanol and ethyl alcohol.
White carbon, calcium carbonate, diatomite, silica flour, mica powder, titanium dioxide, kaolin, pottery can be selected in the filler
At least one of porcelain powder；It is mainly used for improving the works such as intensity, denseness, thixotropy, delustring, uvioresistant, the sterilization of strengthening agent
With；Preferably white carbon；More preferably hydrophobic aerosil.
Organic tin catalyst or titanium complex catalyst can be selected in the catalyst；Preferably titanium complex is catalyzed
Agent.
Dibutyl tin laurate, dibutyltin diacetate, stannous octoate, two can be selected in the organic tin catalyst
In (dodecyl sulphur) dibutyl tin, tin dilaurate dioctyl tin, dialkyl tin dimaleate, two mercaptan tin alkyls at least
It is a kind of.
The metatitanic acid tert-butyl ester, butyl titanate, chelating titanate, load-type Titanium can be selected in the titanium complex catalyst
At least one of acid esters.
Further, the mass fraction of the diluent is preferably 1~5 part.
Further, the filler is preferably gas-phase silica, and mass fraction is 0.3~0.8 part.
Preferably, above-mentioned decayed rock historical relic strengthening agent is obtained by the component reaction for including following mass parts meter：
60~98 parts of esters of silicon acis；
0~30 part of organosilicon compound；
1.2~12.8 parts of deionized waters；
0.01~0.1 part of hydrolyst；
0~6 part of diluent；
0~0.8 part of filler；
0~0.6 part of catalyst.
The structural formula of the organosilicon compound is as follows：
R1-Si-(OR2)3Or (R1,R3)-Si-(OR2)2
Wherein R1、R3Identical or different is respectively alkyl, aryl, alkenyl, aralkyl or alkaryl；R2For methyl or
Ethyl.
Preferably, R1、R3Identical or different is respectively methyl or ethyl.
The present invention also provides a kind of preparation methods of above-mentioned decayed rock historical relic strengthening agent, comprise the following steps：
(1) esters of silicon acis and organosilicon compound are uniformly mixed, are added with stirring water and hydrolyst, 0~40 DEG C
Reaction hydrolysis；
(2) application of vacuum, abjection moisture and the small molecule by-product generated；
(3) diluent, filler and catalyst are added in into system after processing, is stirred evenly to get the decomposed rock of the present invention
Stone historical relic strengthening agent.
The time of step (1) the reaction hydrolysis can be 0.5~10h, and preferably reaction is hydrolyzed into colourless transparent solution.
The solid content of the decayed rock historical relic strengthening agent for the present invention that the above method is prepared is 30~70%.
Esters of silicon acis first carries out partial hydrolysis in step 1 in preparation method of the present invention, generates part small molecule, then passes through vacuum
Processing removes moisture and small-molecule substance, condensation reaction is had again between the product of hydrolysis, so as to control the molecule of condensation product
Amount and solid content, and products therefrom is not finally aqueous.
The decayed rock historical relic strengthening agent of the present invention can be used for the reinforcing and reinforcement of decayed rock historical relic, due to strengthening agent not
Containing moisture, rock historical relic is not destroyed, the mechanical strength of historical relic and water resistance significantly improve after reinforcing.
The present invention is had the following advantages and advantageous effect compared with the prior art：
It 1st, can be rapid after the present invention is contacted using the functional group of hydrolyzable present in strengthening agent with the moisture in air
Generation hydrolysis-condensation reaction generates so as to cause strengthening agent inside and cures crosslinking, forms tridimensional network.This curing agent energy
It effectively permeates and is filled into the hole and crack of decayed rock, be bonded as one the rock of weathering by curing crosslinking,
Improve the intensity of rock historical relic.
2nd, decayed rock historical relic strengthening agent hardening time of the invention can require to adjust according to Specific construction.
3rd, decayed rock historical relic strengthening agent solidification effect of the invention significantly improves.
Specific embodiment
With reference to embodiment, the present invention is described in further detail, but the implementation of the present invention is not limited to this.
Material involved in the following example can be obtained from commercial channel.
The test method of each performance：
The test method of hardening time：The decayed rock strengthening agent prepared with 3.0~5.0g of electronic balance precise,
23 ± 2 DEG C of room temperature is placed in, is cured in the environment of humidity 50 ± 10%, per the state for observing curing agent every other hour, records surface drying
Time.
The test method of the solid content of strengthening agent：The accurate weighing dried and clean measuring cup on assay balance, then with small
Drop bottle is toward 3.0~5.0g samples, then correct amount are added dropwise in measuring cup.The measuring cup for weighing up sample is put into constant temperature oven,
When 105 ± 1 DEG C of constant temperature 8 are small, then at 120 ± 1 DEG C of constant temperature 2 it is small when, taking-up be put into dry vessel, be cooled to room temperature and weigh.
Formula result of calculation as the following formula：
Solid content %=(W1-W2)/W*100%
In formula, W1For dry sample and measuring cup gross weight；W2For measuring cup quality；W is sample mass.
Taking the arithmetic mean of instantaneous value of three parallel tests, test error should not exceed 1% as result of the test.
The esters of silicon acis a used in the present invention：
Component a-1：Methyl silicate；
Component a-2：Silester；
Component a-3：Butyl silicate；
The organic silicon substance b used in the present invention：
Component b：Methyltriethoxysilane；
The diluent c that the present invention uses：
Component c：Absolute ethyl alcohol；
The filler d used in the present invention：
Component d-1：Gas phase hydrophobic silica DM-20S；
Component d-2：Gas phase hydrophilic silicon oxides QS-10；
Component d-3：Ceramic powder；
The catalyst e used in the present invention：
Component e-1：Dibutyl tin laurate；
Component e-2：Dibutyltin diacetate.
Embodiment 1
A kind of decayed rock historical relic strengthening agent is made of following mass parts component, including：96 parts of component a；1.5 parts of group
Divide b；2.4 parts of component c；0 part of component d；0.1 part of component e.Its preparation method includes the following steps：The first step, to reaction
96 parts of component a and 1.5 parts of component b are added in kettle, and is stirred evenly；Second step in the state of stirring, adds into reaction kettle
Enter 2.1 parts deionized water and 0.04 part of hydrolyst, and be stirred to react at 0~40 DEG C, until reaction solution is in colourless
It is transparent, stop reaction；3rd step takes out reaction solution vacuum removal small-molecule substance；4th step adds in 2.4 parts into solution
Diluent c, 0 part of filler d and 0.1 part of catalyst e, stir evenly and are sealed.
Embodiment 2
A kind of decayed rock historical relic strengthening agent is made of following mass parts component, including：90 parts of component a；7.5 parts of group
Divide b；2.3 parts of component c；0 part of component d；0.2 part of component e.Preparation method is the same as embodiment 1.
Embodiment 3
A kind of decayed rock historical relic strengthening agent is made of following mass parts component, including：98 parts of component a；0 part of component
b；1.5 parts of component c；0 part of component d；0.5 part of component e.Preparation method is the same as embodiment 1.
Embodiment 4
A kind of decayed rock historical relic strengthening agent is made of following mass parts component, including：60 parts of component a；30 parts of group
Divide b；5 parts of component c；4.5 parts of component d；0.5 part of component e.Preparation method is the same as embodiment 1.
Embodiment 5
A kind of decayed rock historical relic strengthening agent is made of following mass parts component, including：90 parts of component a；3.5 parts of group
Divide b；6 parts of component c；0 part of component d；0.6 part of component e.Preparation method is the same as embodiment 1.
Embodiment 6
A kind of decayed rock historical relic strengthening agent is made of following mass parts component, including：80 parts of component a；15 parts of group
Divide b；4 parts of component c；0.4 part of component d；0.6 part of component e.Preparation method is the same as embodiment 1.
Embodiment 7
A kind of decayed rock historical relic strengthening agent is made of following mass parts component, including：95 parts of component a；4 parts of component
b；0 part of component c；0.5 part of component d；0.5 part of component e.Preparation method is the same as embodiment 1.
Embodiment 8
A kind of decayed rock historical relic strengthening agent is made of following component, including：60 parts of component a；20 parts of component b；2.8
The component c of part；16 parts of component d；0.6 part of component e.Preparation method is the same as embodiment 1.
Historical relic strengthening agent prepared by the present invention can be configured to different viscosity and solid content, realize to different extent of the destruction
Historical relic repaired and reinforced.From table 1 it follows that different wire feedings differs to the influence degree of strengthening agent viscosity
Sample, but increase the viscosity that filler is all conducive to improve strengthening agent；Hardening time reduces with the increase of catalyst content, simultaneously
The addition of filler is conducive to shorten hardening time；The addition of organic silicon monomer can substantially improve the hydrophobic performance of strengthening agent,
So as to improve the water resistance after historical relic is repaired.The degree that the present invention can be destroyed according to historical relic, prepares and meets relevant art
It is required that strengthening agent product repaired, realize to historical relic reinforcing enhancing.
The specific proportioning (mass parts) of 1 Examples 1 to 8 of table and its performance test results
Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention and from above-described embodiment
Limitation, other any Spirit Essences without departing from the present invention with made under principle change, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (10)
1. a kind of decayed rock historical relic strengthening agent, it is characterised in that obtained by the component reaction for including following mass parts meter：
60~98 parts of esters of silicon acis；
0~30 part of organosilicon compound；
1.2~12.8 parts of deionized waters；
0.01~0.1 part of hydrolyst；
0~6 part of diluent；
0~16 part of filler；
0~0.6 part of catalyst.
2. decayed rock historical relic strengthening agent according to claim 1, it is characterised in that：
The structural formula of the organosilicon compound is as follows：
R1-Si-(OR2)3Or (R1,R3)-Si-(OR2)2
Wherein R1、R3Identical or different is respectively alkyl, aryl, alkenyl, aralkyl or alkaryl；R2For methyl or ethyl.
3. decayed rock historical relic strengthening agent according to claim 2, it is characterised in that in the organosilicon compound：
The alkyl includes methyl, ethyl, propyl, isopropyl, normal-butyl, isobutyl group, sec-butyl, tertiary butyl；
The aryl include phenyl, 1- how base, 2- how base；
The alkenyl includes vinyl, pi-allyl, acrylic, isopropenyl；
The aralkyl includes benzyl, phenethyl；
The alkaryl includes o- tolyl, m- tolyl, p- tolyl, o- ethylbenzene, m- ethylbenzene, p- ethylbenzene
Base.
4. decayed rock historical relic strengthening agent according to claim 1, it is characterised in that：
The esters of silicon acis includes methyl orthosilicate, silester, silicic acid propyl ester, butyl silicate, four (1- Methylethyls) silicic acid
At least one of ester, four phenyl ester of silicic acid, four (2- ethyl-butyls) esters of silicon acis and four (2- ethylhexyls) esters of silicon acis；
The hydrolyst selects aqueous hydrochloric acid solution, aqueous sulfuric acid, aqueous solution of nitric acid, phosphate aqueous solution, formic acid and second
Acid；
The diluent selects at least one of methanol, ethyl alcohol, normal propyl alcohol, isopropanol, n-butanol, isobutanol, ether；
The filler is selected in white carbon, calcium carbonate, diatomite, silica flour, mica powder, titanium dioxide, kaolin, ceramic powder
At least one；
The catalyst selects organic tin catalyst or titanium complex catalyst.
5. decayed rock historical relic strengthening agent according to claim 1, it is characterised in that：The organic tin catalyst choosing
With dibutyl tin laurate, dibutyltin diacetate, stannous octoate, two (dodecyl sulphur) dibutyl tins, tin dilaurate two
At least one of tin octylate, dialkyl tin dimaleate, two mercaptan tin alkyls；
The titanium complex catalyst is selected in the metatitanic acid tert-butyl ester, butyl titanate, chelating titanate, load-type Titanium acid esters
At least one.
6. decayed rock historical relic strengthening agent according to claim 1, it is characterised in that：
The esters of silicon acis is at least one of silester Si-28, Si-32 and Si-40；
The diluent selects at least one of methanol and ethyl alcohol；
The filler selects white carbon；
The catalyst selects titanium complex catalyst.
7. decayed rock historical relic strengthening agent according to claim 1, it is characterised in that：The mass fraction of the diluent is
1~5 part；The filler is gas-phase silica, and mass fraction is 0.3~0.8 part.
8. decayed rock historical relic strengthening agent according to claim 1, it is characterised in that solid content is 30~70%.
9. decayed rock historical relic strengthening agent according to claim 1, it is characterised in that by the group for including following mass parts meter
Divide and be obtained by the reaction：
60~98 parts of esters of silicon acis；
0~30 part of organosilicon compound；
1.2~12.8 parts of deionized waters；
0.01~0.1 part of hydrolyst；
0~6 part of diluent；
0~0.8 part of filler；
0~0.6 part of catalyst.
A kind of 10. preparation method of claim 1~9 any one of them decayed rock historical relic strengthening agent, it is characterised in that bag
Include following steps：
(1) esters of silicon acis and organosilicon compound are uniformly mixed, are added with stirring water and hydrolyst, 0~40 DEG C of reaction
Hydrolysis；
(2) application of vacuum, abjection moisture content and the small molecule by-product generated；
(3) diluent, filler and catalyst are added in into system after processing, stirs evenly the decayed rock text to get the present invention
Object strengthening agent.
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| CN111116112A (en) * | 2019-12-31 | 2020-05-08 | 宁波财经学院 | Preparation method of in-situ soil brick and application of in-situ soil brick prepared by method |
| CN113816768A (en) * | 2021-09-15 | 2021-12-21 | 上海大学 | Method for reinforcing silicate cultural relics by hyperbranched polysiloxane and application |
| CN115088726A (en) * | 2022-07-28 | 2022-09-23 | 四川省文物考古研究院 | Moss-removing bactericidal reagent for stone cultural relics and application thereof |
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| CN103739307A (en) * | 2013-12-13 | 2014-04-23 | 四川大学 | Sandstone stone cultural relic protection material, preparation method and application method |
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| CN115088726A (en) * | 2022-07-28 | 2022-09-23 | 四川省文物考古研究院 | Moss-removing bactericidal reagent for stone cultural relics and application thereof |
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| Publication number | Publication date |
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| CN108084872B (en) | 2020-06-05 |
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