CN106747648A - A kind of preparation method of durable stable type stone protectant - Google Patents
A kind of preparation method of durable stable type stone protectant Download PDFInfo
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- CN106747648A CN106747648A CN201611211668.6A CN201611211668A CN106747648A CN 106747648 A CN106747648 A CN 106747648A CN 201611211668 A CN201611211668 A CN 201611211668A CN 106747648 A CN106747648 A CN 106747648A
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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
- C04B41/46—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 organic materials
- C04B41/48—Macromolecular compounds
- C04B41/4803—Polysaccharides, e.g. cellulose, or derivatives thereof
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
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- Organic Chemistry (AREA)
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Abstract
The present invention relates to a kind of preparation method of durable stable type stone protectant, belong to stone protectant technical field.The present invention is using the hydriopsis cumingii shell for scraping off casting skin, in ball milling, Nacre is obtained after sieving, and mix with deionized water, heating is prepared into mother-of-pearl dispersion liquid, during lactic acid dropped into mother-of-pearl dispersion liquid, filter and concentrate the modified matrix liquid being prepared into, then mix with absolute ethyl alcohol and be placed in beaker, then by calcium oxalate ball milling, sieve to obtain calcium oxalate ball-milled powder, and mix with above-mentioned Liposomal dispersion, it is prepared into durable stable type stone protectant, obtained stone protectant of the invention is by being coated in stone surface, infiltrate into stone material is internally formed diaphragm, stone material is effectively protected.
Description
Technical field
The present invention relates to a kind of preparation method of durable stable type stone protectant, belong to stone protectant technical field.
Background technology
Stone material is widely used in various buildings as one of the most frequently used construction material, but in sunshine, weathering and water erosion etc. certainly
The effect of right factor, stone material can occur lesion, decompose and fragmentation, stone appearance be influenceed, in particular for the facing of TERRAZZO
Color.Especially as industrial development, nowadays the more serious acid rain phenomenon of Some Domestic area appearance, aggravates the journey of stone material etch
Degree.Therefore, prior art is coated in stone surface using stone protectant, contact of the stone material with pollution sources is limited, it is anti-to reach
Water, grease proofing, the purpose such as acid and alkali-resistance.The species of stone surface protective agent is a lot, and classification is not quite similar, and can divide by material property
For：Inorganic surfaces protective agent and organic surface-protective agent；Can be divided into by protection method：Semipermanent is protected（Such as paraffin, silicone oil
Deng）With permanent protection（Such as cold coating）；Can be divided into by mechanism of action：Surface filming type and Seep- Solidifying type；Can by purposes
It is divided into：Surface-protective agent, bottom surface protective agent etc..
The development experience of current stone protectant turpentine oil, paraffin, epoxy, acrylic acid, organosilicon, fluorine-containing osmosis type are prevented
Six stages such as shield agent.Protection of the organosilicon material on stone material is by the chemistry between organosilicon material and stone material inorganic material
Relation determine, because the two chemical constitution is all Si-O keys, under given conditions, the silanol groups of stone surface with it is organic
There is condensation dehydration in silicon molecular radical so that closely combined one between being connected to the silicone molecules on stone product surface
Rise, form organosiloxane hydrophobic film.Although hydrophobic film can stop that moisture enters stone material, steam can in hydrophobic film area
Free permeation, so as to ensure that the gas permeability of stone material.The bond energy of Si-O keys is higher to can reach 422.5KJ/mol, assigns organosilicon
Oxygen alkane protective agent heat endurance higher.But organic silicon stone protective agent, although hydrophobic performance is preferably, what the protective agent was present
Once have the disadvantage that the protective agent film breakage for being coated in stone surface will be difficult to repair so that stone surface forms hole shape corrosion, no
But protection cannot be formed, and have impact on the outward appearance of stone material.
The content of the invention
The present invention solves the technical problem of：For Bartlit protective agent long-term use stability and wearability
Difference, at the same to surrounding environment toxic side effect, and influenceing the problem of the outward appearance of stone material, there is provided one kind passes through hydriopsis cumingii shell
Preparation mother-of-pearl hydrolyzate is milled and hydrolyzed, organic formwork is used as by mother-of-pearl Polysaccharides, calcium oxalate saturated solution is nothing
Machine presoma, acts on stone surface, and stone protecting agent is separated out calcium oxalate, cooperateed with by mother-of-pearl hydrolyzate through spontaneously drying
Effect, penetrates deep into stone material pore interior, under the calcareous and calcium oxalate concerted reaction of mother-of-pearl dissolving, in stone surface shape
Into the method for fine and close protective layer, the present invention utilizes hydriopsis cumingii shell, after ball milling, sieving Nacre, with go from
Sub- water mixing, heating is prepared into mother-of-pearl dispersion liquid, during lactic acid dropped into mother-of-pearl dispersion liquid, after being added dropwise to complete, and filtering
And filtrate is collected, it is prepared into modified matrix liquid after evaporation, then it is placed in beaker with absolute ethyl alcohol etc., after cooling is heated
Mixing, obtained dry particle mixes with phosphate buffer, prepared Liposomal dispersion, then by calcium oxalate ball milling, sieve
Calcium oxalate ball-milled powder, mixes with above-mentioned Liposomal dispersion, is prepared into a kind of durable stable type stone protectant, the present invention
Obtained stone protectant is coated in stone surface by modes such as roller coat, brushing, spraying or immersions, infiltrates into the inside of stone material
Diaphragm is formed, stone material is effectively protected.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
（1）Hydriopsis cumingii shell is chosen, is dried naturally after being cleaned, after shell outer layer casting skin is scraped off with knife, be placed on
3~5h of ball milling under 250~300r/min, crosses 100 mesh sieves, is prepared into Nacre, and then in mass ratio 1:10, by mother-of-pearl
Powder mixes with deionized water stirring, and 25~30min of heating water bath at 45~50 DEG C is prepared into mother-of-pearl dispersion liquid；
（2）In mass ratio 1:5, lactic acid is dropped in the mother-of-pearl dispersion liquid of above-mentioned preparation, it is 85~90 to control dropping temperature
DEG C, time for adding is 55~60min, and after being added dropwise to complete, 25~30min of insulation reaction then stands and is cooled to room temperature, filters
And filtrate is collected, rotation is evaporated to the 1/5 of original volume at 75~80 DEG C, is prepared into modified matrix liquid；
（3）Count by weight, weigh respectively 45~50 parts of modified matrix liquid of above-mentioned preparation, 45~50 parts of absolute ethyl alcohols, 3~
5 parts of polyethylene glycol, 5~8 parts of cholesterol and 8~10 parts of sorbester p18s are placed in beaker, at 55~60 DEG C heating water bath 25~
30min, then stands and is cooled to room temperature, and after 1~2h of stirring mixing, vacuum freeze drying simultaneously collects dry particle, in mass ratio
1:5, dry particle is mixed with the potassium dihydrogen phosphate that pH is 6.8-dipotassium hydrogen phosphate stirring, it is prepared into Liposomal dispersion；
（4）Calcium oxalate is placed in ball grinder, after 3~5h of ball milling under 350~400r/min, 100 mesh sieves is crossed, oxalic acid is collected to obtain
Calcium ball-milled powder, then in mass ratio 1:5, calcium oxalate ball-milled powder is mixed with the Liposomal dispersion stirring of above-mentioned preparation,
After standing 6~8h at room temperature, filtrate is filtered and collected, you can be prepared into a kind of durable stable type stone protectant.
Application process of the invention：The stone material that protective agent first is will be coated cleaned out, then by 130~150mL/m2Use
Stone protectant obtained in the present invention is evenly applied to stone surface by amount, then is placed in dry 20~24h is conserved in ventilated environment,
.After testing, it is 3~5 μm of diaphragms that the obtained protective agent of the present invention can form a thickness in stone surface, and water proofing property is 92
~95%, acid resistance is 58~70%, and resistance to ag(e)ing is 85~88%, even and if long-term being in the outer of stone material under ultraviolet irradiation
See without influence.
The beneficial effects of the invention are as follows：
（1）Stone protectant preparation method is simple prepared by the present invention, no coupling product is free from environmental pollution, and physical and chemical performance is excellent, should
With it is in extensive range and easy to use the characteristics of；
（2）Stone protectant of the invention obtained effectively in the inside of stone material and surface formation overcoat, can make stone material waterproof,
Weather-proof and pollution resistance is significantly improved.
Specific embodiment
Hydriopsis cumingii shell is chosen, is dried naturally after being cleaned, after shell outer layer casting skin is scraped off with knife, be placed on
3~5h of ball milling under 250~300r/min, crosses 100 mesh sieves, is prepared into Nacre, and then in mass ratio 1:10, by mother-of-pearl
Powder mixes with deionized water stirring, and 25~30min of heating water bath at 45~50 DEG C is prepared into mother-of-pearl dispersion liquid；By matter
Amount compares 1:5, lactic acid is dropped in the mother-of-pearl dispersion liquid of above-mentioned preparation, it is 85~90 DEG C, time for adding to control dropping temperature
It is 55~60min, after being added dropwise to complete, 25~30min of insulation reaction then stands and is cooled to room temperature, filters and collect filtrate,
Rotation is evaporated to the 1/5 of original volume at 75~80 DEG C, is prepared into modified matrix liquid；Count by weight, respectively weigh 45~
50 parts of the modified matrix liquid of above-mentioned preparation, 45~50 parts of absolute ethyl alcohols, 3~5 parts of polyethylene glycol, 5~8 parts of cholesterol and 8~10
Part sorbester p18 is placed in beaker, 25~30min of heating water bath at 55~60 DEG C, is then stood and is cooled to room temperature, stirring mixing 1
After~2h, vacuum freeze drying simultaneously collects dry particle, and in mass ratio 1:5, by the biphosphate that dry particle and pH are 6.8
Potassium-dipotassium hydrogen phosphate stirring mixing, is prepared into Liposomal dispersion；Calcium oxalate is placed in ball grinder, in 350~400r/min
After 3~5h of lower ball milling, 100 mesh sieves are crossed, collect to obtain calcium oxalate ball-milled powder, then in mass ratio 1:5, by calcium oxalate ball-milled powder
Mix with the Liposomal dispersion stirring of above-mentioned preparation, after standing 6~8h at room temperature, filter and collect filtrate, you can prepare
Obtain a kind of durable stable type stone protectant.
Example 1
Hydriopsis cumingii shell is chosen, is dried naturally after being cleaned, after shell outer layer casting skin is scraped off with knife, be placed on
Ball milling 3h under 250r/min, crosses 100 mesh sieves, is prepared into Nacre, and then in mass ratio 1:10, by Nacre with go
Ionized water stirring mixing, the heating water bath 25min at 45 DEG C is prepared into mother-of-pearl dispersion liquid；In mass ratio 1:5, lactic acid is dripped
Add in the mother-of-pearl dispersion liquid of above-mentioned preparation, control dropping temperature for 85 DEG C, time for adding is 55min, after being added dropwise to complete,
Insulation reaction 25min, then stands and is cooled to room temperature, filters and collect filtrate, and rotation is evaporated to the 1/ of original volume at 75 DEG C
5, it is prepared into modified matrix liquid；Count by weight, 45 parts of the modified matrix liquid of above-mentioned preparation, 45 parts of anhydrous second are weighed respectively
Alcohol, 3 parts of polyethylene glycol, 5 parts of cholesterol and 8 parts of sorbester p18s are placed in beaker, the heating water bath 25min at 55 DEG C, are then stood
Room temperature is cooled to, after stirring mixing 1h, vacuum freeze drying simultaneously collects dry particle, in mass ratio 1:5, by dry particle and pH
It is 6.8 potassium dihydrogen phosphate-dipotassium hydrogen phosphate stirring mixing, is prepared into Liposomal dispersion；Calcium oxalate is placed in ball grinder,
After ball milling 3h under 350r/min, 100 mesh sieves are crossed, collect to obtain calcium oxalate ball-milled powder, then in mass ratio 1:5, by calcium oxalate
Ball-milled powder mixes with the Liposomal dispersion stirring of above-mentioned preparation, after standing 6h at room temperature, filters and collect filtrate, you can
It is prepared into a kind of durable stable type stone protectant.
The stone material that protective agent first is will be coated cleaned out, then by 130mL/m2Consumption stone material obtained in the present invention is prevented
Shield agent is evenly applied to stone surface, then is placed in dry and conserve 20h in ventilated environment, you can.After testing, the present invention is obtained anti-
It is 3 μm of diaphragms that shield agent can form a thickness in stone surface, and water proofing property is 92%, and acid resistance is 58%, and resistance to ag(e)ing is 85%,
Even and if the long-term outward appearance for being in stone material under ultraviolet irradiation is without influence.
Example 2
Hydriopsis cumingii shell is chosen, is dried naturally after being cleaned, after shell outer layer casting skin is scraped off with knife, be placed on
Ball milling 5h under 300r/min, crosses 100 mesh sieves, is prepared into Nacre, and then in mass ratio 1:10, by Nacre with go
Ionized water stirring mixing, the heating water bath 30min at 50 DEG C is prepared into mother-of-pearl dispersion liquid；In mass ratio 1:5, lactic acid is dripped
Add in the mother-of-pearl dispersion liquid of above-mentioned preparation, control dropping temperature for 90 DEG C, time for adding is 60min, after being added dropwise to complete,
Insulation reaction 30min, then stands and is cooled to room temperature, filters and collect filtrate, and rotation is evaporated to the 1/ of original volume at 80 DEG C
5, it is prepared into modified matrix liquid；Count by weight, 50 parts of the modified matrix liquid of above-mentioned preparation, 50 parts of anhydrous second are weighed respectively
Alcohol, 5 parts of polyethylene glycol, 8 parts of cholesterol and 10 parts of sorbester p18s are placed in beaker, the heating water bath 30min at 60 DEG C, are then stood
Room temperature is cooled to, after stirring mixing 2h, vacuum freeze drying simultaneously collects dry particle, in mass ratio 1:5, by dry particle and pH
It is 6.8 potassium dihydrogen phosphate-dipotassium hydrogen phosphate stirring mixing, is prepared into Liposomal dispersion；Calcium oxalate is placed in ball grinder,
After ball milling 5h under 400r/min, 100 mesh sieves are crossed, collect to obtain calcium oxalate ball-milled powder, then in mass ratio 1:5, by calcium oxalate
Ball-milled powder mixes with the Liposomal dispersion stirring of above-mentioned preparation, after standing 8h at room temperature, filters and collect filtrate, you can
It is prepared into a kind of durable stable type stone protectant.
The stone material that protective agent first is will be coated cleaned out, then by 150mL/m2Consumption stone material obtained in the present invention is prevented
Shield agent is evenly applied to stone surface, then is placed in dry and conserve 24h in ventilated environment, you can.After testing, the present invention is obtained anti-
It is 5 μm of diaphragms that shield agent can form a thickness in stone surface, and water proofing property is 95%, and acid resistance is 70%, and resistance to ag(e)ing is 88%,
Even and if the long-term outward appearance for being in stone material under ultraviolet irradiation is without influence.
Example 3
Hydriopsis cumingii shell is chosen, is dried naturally after being cleaned, after shell outer layer casting skin is scraped off with knife, be placed on
Ball milling 4h under 275r/min, crosses 100 mesh sieves, is prepared into Nacre, and then in mass ratio 1:10, by Nacre with go
Ionized water stirring mixing, the heating water bath 28min at 48 DEG C is prepared into mother-of-pearl dispersion liquid；In mass ratio 1:5, lactic acid is dripped
Add in the mother-of-pearl dispersion liquid of above-mentioned preparation, control dropping temperature for 88 DEG C, time for adding is 58min, after being added dropwise to complete,
Insulation reaction 28min, then stands and is cooled to room temperature, filters and collect filtrate, and rotation is evaporated to the 1/ of original volume at 78 DEG C
5, it is prepared into modified matrix liquid；Count by weight, 48 parts of the modified matrix liquid of above-mentioned preparation, 48 parts of anhydrous second are weighed respectively
Alcohol, 4 parts of polyethylene glycol, 7 parts of cholesterol and 9 parts of sorbester p18s are placed in beaker, the heating water bath 28min at 58 DEG C, are then stood
Room temperature is cooled to, after stirring mixing 2h, vacuum freeze drying simultaneously collects dry particle, in mass ratio 1:5, by dry particle and pH
It is 6.8 potassium dihydrogen phosphate-dipotassium hydrogen phosphate stirring mixing, is prepared into Liposomal dispersion；Calcium oxalate is placed in ball grinder,
After ball milling 4h under 375r/min, 100 mesh sieves are crossed, collect to obtain calcium oxalate ball-milled powder, then in mass ratio 1:5, by calcium oxalate
Ball-milled powder mixes with the Liposomal dispersion stirring of above-mentioned preparation, after standing 7h at room temperature, filters and collect filtrate, you can
It is prepared into a kind of durable stable type stone protectant.
The stone material that protective agent first is will be coated cleaned out, then by 140mL/m2Consumption stone material obtained in the present invention is prevented
Shield agent is evenly applied to stone surface, then is placed in dry and conserve 22h in ventilated environment, you can.After testing, the present invention is obtained anti-
It is 4 μm of diaphragms that shield agent can form a thickness in stone surface, and water proofing property is 94%, and acid resistance is 64%, and resistance to ag(e)ing is 87%,
Even and if the long-term outward appearance for being in stone material under ultraviolet irradiation is without influence.
Claims (1)
1. a kind of preparation method of durable stable type stone protectant, it is characterised in that specific preparation process is：
（1）Hydriopsis cumingii shell is chosen, is dried naturally after being cleaned, after shell outer layer casting skin is scraped off with knife, be placed on
3~5h of ball milling under 250~300r/min, crosses 100 mesh sieves, is prepared into Nacre, and then in mass ratio 1:10, by mother-of-pearl
Powder mixes with deionized water stirring, and 25~30min of heating water bath at 45~50 DEG C is prepared into mother-of-pearl dispersion liquid；
（2）In mass ratio 1:5, lactic acid is dropped in the mother-of-pearl dispersion liquid of above-mentioned preparation, it is 85~90 to control dropping temperature
DEG C, time for adding is 55~60min, and after being added dropwise to complete, 25~30min of insulation reaction then stands and is cooled to room temperature, filters
And filtrate is collected, rotation is evaporated to the 1/5 of original volume at 75~80 DEG C, is prepared into modified matrix liquid；
（3）Count by weight, weigh respectively 45~50 parts of modified matrix liquid of above-mentioned preparation, 45~50 parts of absolute ethyl alcohols, 3~
5 parts of polyethylene glycol, 5~8 parts of cholesterol and 8~10 parts of sorbester p18s are placed in beaker, at 55~60 DEG C heating water bath 25~
30min, then stands and is cooled to room temperature, and after 1~2h of stirring mixing, vacuum freeze drying simultaneously collects dry particle, in mass ratio
1:5, dry particle is mixed with the potassium dihydrogen phosphate that pH is 6.8-dipotassium hydrogen phosphate stirring, it is prepared into Liposomal dispersion；
（4）Calcium oxalate is placed in ball grinder, after 3~5h of ball milling under 350~400r/min, 100 mesh sieves is crossed, oxalic acid is collected to obtain
Calcium ball-milled powder, then in mass ratio 1:5, calcium oxalate ball-milled powder is mixed with the Liposomal dispersion stirring of above-mentioned preparation,
After standing 6~8h at room temperature, filtrate is filtered and collected, you can be prepared into a kind of durable stable type stone protectant.
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| CN201611211668.6A CN106747648A (en) | 2016-12-25 | 2016-12-25 | A kind of preparation method of durable stable type stone protectant |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611211668.6A CN106747648A (en) | 2016-12-25 | 2016-12-25 | A kind of preparation method of durable stable type stone protectant |
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| CN106747648A true CN106747648A (en) | 2017-05-31 |
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| CN201611211668.6A Pending CN106747648A (en) | 2016-12-25 | 2016-12-25 | A kind of preparation method of durable stable type stone protectant |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107281088A (en) * | 2017-07-13 | 2017-10-24 | 成都新柯力化工科技有限公司 | A kind of Rice oil face cream and preparation method thereof |
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| CN1772713A (en) * | 2005-10-12 | 2006-05-17 | 浙江大学 | Surface bionic protection method of stone material and lithical cultural relic |
| CN101139215A (en) * | 2007-08-03 | 2008-03-12 | 浙江大学 | Calcium carbonate biomineralization reinforcing method for calcium carbonate type stone cultural relics |
| CN104706567A (en) * | 2015-03-31 | 2015-06-17 | 广西还珠海洋生物科技有限公司 | Method for extracting pearl fetal sac liquid from pearl fetal sac of mother pearl shellfish and product thereby |
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2016
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| CN1334149A (en) * | 2000-07-14 | 2002-02-06 | 浙江大学 | Surface protecting method for Ca-contained rock and cultural stone relics |
| CN1772713A (en) * | 2005-10-12 | 2006-05-17 | 浙江大学 | Surface bionic protection method of stone material and lithical cultural relic |
| CN101139215A (en) * | 2007-08-03 | 2008-03-12 | 浙江大学 | Calcium carbonate biomineralization reinforcing method for calcium carbonate type stone cultural relics |
| CN104706567A (en) * | 2015-03-31 | 2015-06-17 | 广西还珠海洋生物科技有限公司 | Method for extracting pearl fetal sac liquid from pearl fetal sac of mother pearl shellfish and product thereby |
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Cited By (1)
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| CN107281088A (en) * | 2017-07-13 | 2017-10-24 | 成都新柯力化工科技有限公司 | A kind of Rice oil face cream and preparation method thereof |
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Application publication date: 20170531 |