CN106172492A - A kind of rare cultural relics, literature and history archives, calligraphy and painting protecting agent preparation method and applications - Google Patents
A kind of rare cultural relics, literature and history archives, calligraphy and painting protecting agent preparation method and applications Download PDFInfo
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- CN106172492A CN106172492A CN201610543239.2A CN201610543239A CN106172492A CN 106172492 A CN106172492 A CN 106172492A CN 201610543239 A CN201610543239 A CN 201610543239A CN 106172492 A CN106172492 A CN 106172492A
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/16—Heavy metals; Compounds thereof
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N41/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a sulfur atom bound to a hetero atom
- A01N41/02—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a sulfur atom bound to a hetero atom containing a sulfur-to-oxygen double bond
- A01N41/04—Sulfonic acids; Derivatives thereof
- A01N41/06—Sulfonic acid amides
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/48—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with two nitrogen atoms as the only ring hetero atoms
- A01N43/50—1,3-Diazoles; Hydrogenated 1,3-diazoles
- A01N43/52—1,3-Diazoles; Hydrogenated 1,3-diazoles condensed with carbocyclic rings, e.g. benzimidazoles
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/72—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms
- A01N43/74—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms five-membered rings with one nitrogen atom and either one oxygen atom or one sulfur atom in positions 1,3
- A01N43/78—1,3-Thiazoles; Hydrogenated 1,3-thiazoles
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Abstract
The invention discloses a kind of rare cultural relics, literature and history archives, calligraphy and painting protecting agent preparation method and applications, it is made up of following components proportioning by weight: remove silicate cement, fatty acyl monoethanolamine polyoxyethylene ether, methyl nadic anhydride, N methyl N nitro-p-toluenesulfonamide, 4 nitrophthalimide, 1 amino 2 tectoquinone, 4 bromine 1 amino anthraquinones 2 sulfonic acid, to methoxybenzene, gold nano particulate, diphenyl methane, dimercaptosuccinic acid, 2, 6 diisopropyl phenylisocyanates, 2 pairs of benzotrifluoride 4 methyl 5 thiazole ethyl formates, methyl 1H benzimidazole 2 aminocarbamic acid ester, to chlorine α Bromophenylacetic acid.This invention advantage is: this method prevent protective agent saponification, reduces elaioleucite surface tension so that the attachment of archives surface protectant is more firm；This protective agent have stable chemical nature, be suitable for wide, protected effect is good, to archives not damaged, the advantage of clean surface.
Description
Technical field
The invention belongs to books, document, calligraphy and painting protecting field, particularly relate to a kind of rare cultural relics, literature and history archives, calligraphy and painting guarantor
Protect agent preparation method and applications.
Background technology
Many archives do not reach constant temperature and humidity due to storehouse maintaining requirement, and archive content easily grows harmful organism, often
Occur have Trogoderma variabile Ballion, casting skin khapra beetle, Lepismae saccharinae, lasioderma serricorne, archives steal worm etc., they can with the straw pulp in archives of paper quality,
The celluloses such as wood pulp and amylum adhesive are foodstuff, directly destroy profile entity, very harmful.The adaptation to environment of these insects
Property very strong, under more severe living environment, also can survive for a long time.As a example by khapra beetle, from low temperature, the dry January to
The May that temperature rises, can survive all the time, conceal in corner motionless when the temperature is low, the most movable when temperature is higher.
Archives insect fertility is very strong, and once condition maturity will be laid eggs in a large number, and storage area insect pest once occurs,
It is difficult to kill.
Eliminating the harmful organism in archives, conventional files department commonly uses pest control with insecticide method, typically have stomach poison, contact insecticide,
Fumigant three class, wherein conventional fumigant has bromomethane, oxirane and hydrogen phosphide etc., and conventional physical method for killing pests has low
Temperature frozen insecticide, gamma-ray irradiation parasite killing, controlled atmosphere insecticidal technology etc..
The shortcoming of pest control with insecticide maximum is to produce environment to pollute, and such as hydrogen phosphide parasite killing, it is the biggest the killing of a kind of toxicity
Worm agent, the harm to human body is the most serious.Grain department test shows, the grain physics to hydrogen phosphide during fumigant insect killing
Although absorption can quickly be resolved when scattered gas, but the grain hydrogen phosphide after fumigating still has certain residual.
Used chemical agent parasite killing to affect environmental and human health impacts in the past, and used vacuum nitrogen parasite killing container batch little, adopt
Carrying out parasite killing by Refrigeration Technique, need to move archives, some historical archives, due to of the remote past, are typically not suitable for moving, after moving
Affecting achive keeping quality, archival quality also can be had a negative impact by the drastic change of temperature.
Summary of the invention
In order to solve the deficiencies in the prior art, the present invention provides a kind of rare cultural relics, literature and history archives, calligraphy and painting protecting agent, its
It is characterised by, is made up of following components proportioning by weight: go silicate cement 228.562～453.27 parts, fatty acyl list second
Hydramine polyoxyethylene ether 20.605～62.307 parts, methyl nadic anhydride 23.504～132.222 parts, N-first
Base-N-nitro-p-toluenesulfonamide 19.511～36.484 parts, 4-nitrophthalimide 22.596～79.47 parts,
1-amino-2-methyl anthraquinone 25.794～86.228 parts, 4-bromo-1-amino anthraquinones-2-sulfonic acid 22.854～45.148 parts, to first
Epoxide benzene 19.713～64.715 parts, gold nano particulate 27.52～82.476 parts, diphenyl methane 20.415～62.162 parts,
Dimercaptosuccinic acid 10.524～53.327 parts, 2,6-diisopropyl phenylisocyanates 11.359～47.16 parts, 2-is to fluoroform
Benzene-4-methyl-5-thiazole formic acid ethyl ester 22.914～62.835 parts, methyl isophthalic acid H-benzimidazolyl-2 radicals-base-carbamate
29.433～73.610 parts, mass concentration be 19.967ppm～286.0ppm to chloro-alpha-brominated phenylacetic acid 52.296～
106.355 part.
Further, it is made up of following components proportioning by weight: remove silicate cement 229.562～452.27 parts, fat
Fat acyl monoethanolamine polyoxyethylene ether 21.605～61.307 parts, methyl nadic anhydride 24.504～131.222
Part, N-methyl-N-nitro-p-toluenesulfonamide 20.511～35.484 parts, 4-nitrophthalimide 23.596～
78.47 parts, 1-amino-2-methyl anthraquinone 26.794～85.228 parts, 4-bromo-1-amino anthraquinones-2-sulfonic acid 23.854～
44.148 parts, to methoxybenzene 20.713～63.715 parts, gold nano particulate 28.52～81.476 parts, diphenyl methane
21.415～61.162 parts, dimercaptosuccinic acid 11.524～52.327 parts, 2,6-diisopropyl phenylisocyanates 12.359～
46.16 parts, 2-to benzotrifluoride-4-methyl-5-thiazole formic acid ethyl ester 23.914～61.835 parts, methyl isophthalic acid H-benzimidazole-
2-base-carbamate 30.433～72.610 parts, mass concentration be 20.967ppm～285.0ppm to chloro-alpha-brominated benzene
Acetic acid 53.296～105.355 parts.
Further, the invention also discloses a kind of rare cultural relics, literature and history archives, the preparation method of calligraphy and painting protecting agent, press
Weight portion meter, comprises the steps:
1st step: in esterification vertical response still, add and remove silicate cement and fatty acyl monoethanolamine polyoxyethylene ether, start ester
Changing the blender in vertical response still, setting speed is 21.849rpm～67.706rpm, starts in esterification vertical response still
Double-stage heating device, makes temperature rise to 36.586 DEG C～37.420 DEG C, adds methyl nadic anhydride and stirs,
Carry out enzyme catalysis fluorescentization to react 13.136～24.825 minutes, add N-methyl-N-nitro-p-toluenesulfonamide, be passed through stream
Amount is 12.332m3/ min～53.690m3The chlorine 0.21 of/min～0.86 hour；Add in esterification vertical response still afterwards
4-nitrophthalimide, is again started up the double-stage heating device being esterified in vertical response still, makes temperature rise to 53.586
DEG C～86.420 DEG C, be incubated 13.332～24.359 minutes, add 1-amino-2-methyl anthraquinone, adjust esterification vertical response still
The pH value of middle solution is 4.8746～8.9962, is incubated 13.332～253.359 minutes；
2nd step: another depletion nanoparticle, by gold nano particulate ultrasonic Treatment under power is 5.531KW～10.97359KW
0.19～0.86 hour, attrition grinding, and by 408.748～508.980 eye mesh screens；Gold nano particulate is joined another
In esterification vertical response still, add the diphenyl methane dispersion gold nano that mass concentration is 23.986ppm～253.386ppm micro-
Grain, starts the double-stage heating device in esterification vertical response still, makes solution temperature at 4.8332 × 10 DEG C～8.9420 × 10 DEG C
Between, start the blender in esterification vertical response still, and with 4.8586 × 102Rpm～8.9706 × 102The speed of rpm is stirred
Mix, adjust pH value between 4.81～8.9359, insulated and stirred 5.53 × 10-1～10.97 × 10-1Hour；Stopped reaction afterwards
Stand 5.53 × 10～10.97 × 10 minutes, go the removal of impurity；Suspension is added 2-to benzotrifluoride-4-methyl-5-thiazole first
Acetoacetic ester, adjustment pH value, between 1.332～2.690, forms precipitate and spends silicate cement eluting, by centrifuge at rotating speed
4.748×103Rpm～9.980 × 103Solid content is obtained, 2.386 × 10 under rpm2DEG C～3.706 × 102Do at a temperature of DEG C
Dry, cross 8.748 × 10 after grinding3～9.980 × 103Mesh sieve, standby；
3rd step: separately take 4-bromo-1-amino anthraquinones-2-sulfonic acid, methoxybenzene and the 2nd step are processed after gold nano particulate, mixing is all
Use X to penetrate top dorsad after even and penetrate irradiation, X penetrate top dorsad penetrate the energy of irradiation be 10.358MeV～38.370MeV, dosage be
58.937kGy～98.624kGy, irradiation time are 22.438～47.541 minutes, obtain the 4-bromo-1-amino anthracene that character changes
Quinone-2-sulfonic acid, to methoxybenzene and gold nano particulate mixture；By bromo-for 4-1-amino anthraquinones-2-sulfonic acid, to methoxybenzene and
Gold nano particulate mixture is placed in another esterification vertical response still, starts the double-stage heating device in esterification vertical response still,
Design temperature 21.746 DEG C～67.690 DEG C, start esterification vertical response still in blender, rotating speed be 13.332rpm～
408.1rpm, pH are adjusted between 4.8358～8.9370, are dehydrated 22.706～36.136 minutes, standby；
4th step: 4-bromo-1-amino anthraquinones-2-sulfonic acid that the character that the 3rd step obtained changes, micro-to methoxybenzene and gold nano
Grain mix homogeneously, adds in the diphenyl methane that mass concentration is 23.986ppm～253.386ppm, and stream adds to the 1st step
In esterification vertical response still, flow acceleration is 158.310mL/min～886.146mL/min；Start esterification vertical response still to stir
Mixing machine, setting speed is 27.844rpm～67.821rpm；Stir 4.8849～8.9370 minutes；Add dimercapto succinum
Acid, starts the double-stage heating device in esterification vertical response still, is warming up to 57.17 DEG C～94.679 DEG C, and pH is adjusted to 4.8986
～between 8.9386, being passed through chlorine ventilation is 12.849m3/ min～53.825m3/ min, insulation stands 47.268～77.615
Minute；Being again started up being esterified vertical response still blender, rotating speed is 22.710rpm～67.526rpm, adds 2,6-diisopropyl
Phenylisocyanate so that it is the hydrophilic/hydrophobic single threshold of reactant liquor is 5.531～10.97359, and make pH be adjusted to 4.817～
Between 8.9679, insulation stands 46.680～86.790 minutes；
5th step: starting the blender in esterification vertical response still, setting speed is 19.521rpm～86.23rpm, while stirring
In esterification vertical response still, add 2-benzotrifluoride-4-methyl-5-thiazole formic acid ethyl ester, startup are esterified in vertical response still
Double-stage heating device, set esterification vertical response still in temperature as 4.780 × 102DEG C～9.195 × 102DEG C, insulation
After 46.680～86.790 minutes, adding methyl isophthalic acid H-benzimidazolyl-2 radicals-base-carbamate, enzyme catalysis fluorescentization is reacted
13.136～24.690 minutes；Add afterwards chloro-alpha-brominated phenylacetic acid, start the double-stage heating dress in esterification vertical response still
Put, set esterification vertical response still in temperature as 97.780 DEG C～153.195 DEG C, pH adjust to 4.8849～8.9825 it
Between, pressure is 0.19230MPa～0.2830MPa, and the response time is 0.412～0.937 hour；It is depressurized to 0MPa afterwards, cooling
To 54.1917 DEG C～59.19386 DEG C of dischargings, i.e. obtain a kind of rare cultural relics, literature and history archives, calligraphy and painting protecting agent.
Further, the particle diameter of described gold nano particulate is 27.27 μm～37.307 μm.
Further, the invention also discloses a kind of rare cultural relics, literature and history archives, the application of calligraphy and painting protecting agent；This business
It is mainly used in the application in processing for the protection containing books, document with books, document preservation.
Further, described books, document be sudd document, mud plate document, Corii Caprae seu Ovis document, the inscriptions on bones or tortoise shells offer, inscription on ancient bronze objects document,
At least one in letter wooden tablets or slips for writing document, stone inscription document, fine silk silks document.
Further, described a kind of rare cultural relics, literature and history archives, calligraphy and painting protecting agent and inert diluent with the use of, one
Kind of rare cultural relics, literature and history archives, calligraphy and painting protecting agent and inert diluent fit quality ratio are for 1:448.222～888.484；Described
Inert diluent is: 1. 5-amino-2-[2-[4-(4,5-dihydro-3-methyl-5-oxo-1H-pyrazol-1-yl)-2-sulfophenyl]
Vinyl]-benzenesulfonic acid, 2. 4-[4-[[3-[(ethylphenyl amino) sulfonyl]-4-aminomethyl phenyl] azo]-4,5-dihydro-3-
Methyl-5-oxygen-1H-pyrazol-1-yl] one in benzenesulfonic acid, 3. three kinds of binary copolymerization chlorine ether, described inert diluent is common
Commercial goods.
A kind of rare cultural relics, literature and history archives, calligraphy and painting protecting agent preparation method and applications disclosed in patent of the present invention, it is excellent
Point is:
(1) a kind of rare cultural relics, literature and history archives, calligraphy and painting protecting agent of the present invention are being used, it is possible to kill harmful organism, will not
Archives, books, data quality are produced any impact, human body is not had any infringement yet；
(2) a kind of rare cultural relics of the present invention, literature and history archives, calligraphy and painting protecting agent can be substantially reduced protective agent at archives, figure
Surface tension on book data surface, thus produce the multiple actions such as lubrication, infiltration, emulsifying, dispersion, so that archives, figure
Book data surface is protected；
(3) a kind of rare cultural relics of the present invention, literature and history archives, calligraphy and painting protecting agent have stable chemical nature, are suitable for wide, pH value
Scope is wide, adhesion-tight rate high, protected effect is good, is not limited by archives, books, data quantity and place, no matter archives, figure
Book, data quantity, can realize once completing, not limited by any external condition, substantially increase archives, figure
The safety coefficient of book, data keeping, reduces the labor intensity of administrator.
(4) a kind of rare cultural relics of the present invention, literature and history archives, calligraphy and painting protecting agent will not produce precipitation after using,
Surrounding enviroment will not be polluted；Apply a kind of rare cultural relics, literature and history archives, calligraphy and painting protecting agent of the present invention, equipment
Requirement is simple, operation cost is low.
Accompanying drawing explanation
Fig. 1 is that a kind of rare cultural relics, literature and history archives, calligraphy and painting protecting agent are real under differential responses time conditions in testing experiment
Execute example and reference examples harmful organism fatality rate variation diagram.
Fig. 2 is that a kind of rare cultural relics, literature and history archives, calligraphy and painting protecting agent are real under differential responses time conditions in testing experiment
Execute example and reference examples protective agent coefficient of stabilization variation diagram.
Fig. 3 is that a kind of rare cultural relics, literature and history archives, calligraphy and painting protecting agent are real under differential responses time conditions in testing experiment
Execute document regeneration rate variation diagram after example uses with reference examples.
Detailed description of the invention
Following example further illustrate present disclosure, but should not be construed as limitation of the present invention.Without departing substantially from
In the case of present invention spirit and essence, the amendment that the inventive method, step or condition are made and replacement, belong to the present invention
Scope.If not specializing, the conventional means that technological means used in embodiment is well known to those skilled in the art.
Embodiment 1
A kind of rare cultural relics, literature and history archives, calligraphy and painting protecting agent of the present invention is prepared according to following steps, and by weight:
1st step: in esterification vertical response still, add and remove silicate cement 228.562 parts, fatty acyl monoethanolamine polyoxyethylene ether
20.605 parts, starting the blender in esterification vertical response still, setting speed is 21.849rpm, starts esterification vertical response still
In double-stage heating device, make temperature rise to 36.586 DEG C, add methyl nadic anhydride 23.504 parts stirring all
Even, carry out enzyme catalysis fluorescentization and react 13.136 minutes, add N-methyl-N-nitro-p-toluenesulfonamide 19.511 parts, logical
Inbound traffics are 12.332m3The chlorine of/min 0.21 hour；4-nitro phthalyl is added afterwards in esterification vertical response still
Imines 22.596 parts, is again started up the double-stage heating device being esterified in vertical response still, makes temperature rise to 53.586 DEG C, insulation
13.332 minutes, adding 1-amino-2-methyl anthraquinone 25.794 parts, adjusting the pH value of solution in esterification vertical response still is
4.8746, it is incubated 13.332 minutes；
2nd step: another depletion nanoparticle 27.52 parts, by little for gold nano particulate ultrasonic Treatment 0.19 under power is 5.531KW
Time, attrition grinding, and by 408.748 eye mesh screens；Gold nano particulate is joined in another esterification vertical response still, add
Mass concentration is the diphenyl methane 20.415 parts of 23.986ppm, disperses gold nano particulate, starts in esterification vertical response still
Double-stage heating device, make solution temperature between 4.8332 × 10 DEG C, start esterification vertical response still in blender, and with
4.8586×102Rpm speed stirring, adjust pH value between 4.81, insulated and stirred 5.53 × 10-1Hour；Stop anti-afterwards
5.53 × 10 minutes should be stood, go the removal of impurity；Suspension is added 2-to benzotrifluoride-4-methyl-5-thiazole formic acid ethyl ester
22.914 parts, adjustment pH value, between 1.332, forms precipitate and spends silicate cement eluting, by centrifuge at rotating speed 4.748
×103Solid content is obtained, 2.386 × 10 under rpm2It is dried at a temperature of DEG C, after grinding, crosses 8.748 × 103Mesh sieve, standby；
3rd step: after separately taking 4-bromo-1-amino anthraquinones-2-sulfonic acid 22.854 parts, methoxybenzene 19.713 parts and the 2nd step being processed
Gold nano particulate 27.52 parts, uses X to penetrate top dorsad and penetrates irradiation after mix homogeneously, X penetrates top dorsad and penetrates the energy of irradiation and is
10.358MeV, dosage are 58.937kGy, irradiation time is 22.438 minutes, obtain character change 4-bromo-1-amino anthraquinones-
2-sulfonic acid, to methoxybenzene and gold nano particulate mixture；By bromo-for 4-1-amino anthraquinones-2-sulfonic acid, to methoxybenzene and Jenner
Rice particle mixture is placed in another esterification vertical response still, starts the double-stage heating device in esterification vertical response still, sets
Temperature 21.746 DEG C, starts the blender in esterification vertical response still, and rotating speed is that 13.332rpm, pH are adjusted between 4.8358,
It is dehydrated 22.706 minutes, standby；
4th step: 4-bromo-1-amino anthraquinones-2-sulfonic acid that the character that the 3rd step obtained changes, micro-to methoxybenzene and gold nano
Grain mix homogeneously, adds in the diphenyl methane 20.415 parts that mass concentration is 23.986ppm, and stream adds to the esterification of the 1st step
In vertical response still, flow acceleration is 158.310mL/min；Starting esterification vertical response still blender, setting speed is
27.844rpm；Stir 4.8849 minutes；Adding dimercaptosuccinic acid 10.524 parts, it is double that startup is esterified in vertical response still
Level heater, is warming up to 57.17 DEG C, and pH is adjusted between 4.8986, and being passed through chlorine ventilation is 12.849m3/ min, insulation
Stand 47.268 minutes；Being again started up being esterified vertical response still blender, rotating speed is 22.710rpm, adds 2,6-diisopropyl
Phenylisocyanate 11.359 parts so that it is the hydrophilic/hydrophobic single threshold of reactant liquor is 5.531, and make pH be adjusted to 4.817 it
Between, insulation stands 46.680 minutes；
5th step: starting the blender in esterification vertical response still, setting speed is 19.521rpm, vertical to esterification while stirring
Reactor adds 2-benzotrifluoride-4-methyl-5-thiazole formic acid ethyl ester 22.914 parts, startup are esterified in vertical response still
Double-stage heating device, sets the temperature in esterification vertical response still as 4.780 × 102DEG C, after being incubated 46.680 minutes, add first
Base-1H-benzimidazolyl-2 radicals-base-carbamate 29.433 parts, carries out enzyme catalysis fluorescentization and reacts 13.136 minutes；Add afterwards
Enter 19.967ppm to chloro-alpha-brominated phenylacetic acid 52.296 parts, start the double-stage heating device in esterification vertical response still, if
Surely the temperature in esterification vertical response still is 97.780 DEG C, and pH adjusts between 4.8849, and pressure is 0.19230MPa, during reaction
Between be 0.412 hour；Be depressurized to 0MPa afterwards, be cooled to 54.1917 DEG C of dischargings, i.e. obtain a kind of rare cultural relics, literature and history archives,
Calligraphy and painting protecting agent.
The particle diameter of wherein said gold nano particulate is 27.27 μm.
In the application, described a kind of rare cultural relics, literature and history archives, calligraphy and painting protecting agent needs coordinate with inert diluent makes
With, a kind of rare cultural relics, literature and history archives, calligraphy and painting protecting agent and inert diluent fit quality ratio for 1:448.222；Described inertia
Diluent is: 5-amino-2-[2-[4-(4,5-dihydro-3-methyl-5-oxo-1H-pyrazol-1-yl)-2-sulfophenyl] ethylene
Base]-benzenesulfonic acid, described inert diluent 5-amino-2-[2-[4-(4,5-dihydro-3-methyl-5-oxo-1H-pyrazoles-1-
Base)-2-sulfophenyl] vinyl]-benzenesulfonic acid is common commercial goods.
Embodiment 2
A kind of rare cultural relics, literature and history archives, calligraphy and painting protecting agent of the present invention is prepared according to following steps, and by weight:
1st step: in esterification vertical response still, add and remove silicate cement 453.27 parts, fatty acyl monoethanolamine polyoxyethylene ether
62.307 parts, starting the blender in esterification vertical response still, setting speed is 67.706rpm, starts esterification vertical response still
In double-stage heating device, make temperature rise to 37.420 DEG C, add methyl nadic anhydride 132.222 parts stirring all
Even, carry out enzyme catalysis fluorescentization and react .24.825 minute, add N-methyl-N-nitro-p-toluenesulfonamide 36.484 parts, logical
Inbound traffics are 53.690m3The chlorine of/min 0.86 hour；4-nitro phthalyl is added afterwards in esterification vertical response still
Imines 79.47 parts, is again started up the double-stage heating device being esterified in vertical response still, makes temperature rise to 86.420 DEG C, insulation
24.359 minutes, adding 1-amino-2-methyl anthraquinone 86.228 parts, adjusting the pH value of solution in esterification vertical response still is
8.9962, it is incubated 253.359 minutes；
2nd step: another depletion nanoparticle 82.476 parts, by gold nano particulate ultrasonic Treatment under power is 10.97359KW
0.86 hour, attrition grinding, and by 508.980 eye mesh screens；Gold nano particulate is joined another esterification vertical response still
In, add the diphenyl methane 62.162 parts that mass concentration is 253.386ppm, disperse gold nano particulate, start esterification vertical instead
Answer the double-stage heating device in still, make solution temperature between 8.9420 × 10 DEG C, start the stirring in esterification vertical response still
Machine, and with 8.9706 × 102Rpm speed stirring, adjust pH value between 8.9359, insulated and stirred 10.97 × 10-1Hour；
Stopped reaction stands 10.97 × 10 minutes afterwards, goes the removal of impurity；Suspension is added 2-to benzotrifluoride-4-methyl-5-thiazole
Ethyl formate 62.835 parts, adjustment pH value, between 2.690, is formed precipitate and spends silicate cement eluting, existed by centrifuge
Rotating speed 9.980 × 103Solid content is obtained, 3.706 × 10 under rpm2It is dried at a temperature of DEG C, after grinding, crosses 9.980 × 103Mesh sieve,
Standby；
3rd step: after separately taking 4-bromo-1-amino anthraquinones-2-sulfonic acid 45.148 parts, methoxybenzene 64.715 parts and the 2nd step being processed
Gold nano particulate 82.476 parts, uses X to penetrate top dorsad and penetrates irradiation after mix homogeneously, X penetrates top dorsad and penetrates the energy of irradiation and is
38.370MeV, dosage are 98.624kGy, irradiation time is 47.541 minutes, obtain character change 4-bromo-1-amino anthraquinones-
2-sulfonic acid, to methoxybenzene and gold nano particulate mixture；By bromo-for 4-1-amino anthraquinones-2-sulfonic acid, to methoxybenzene and Jenner
Rice particle mixture is placed in another esterification vertical response still, starts the double-stage heating device in esterification vertical response still, sets
Temperature 67.690 DEG C, starts the blender in esterification vertical response still, and rotating speed is that 408.1rpm, pH are adjusted between 8.9370,
It is dehydrated 36.136 minutes, standby；
4th step: 4-bromo-1-amino anthraquinones-2-sulfonic acid that the character that the 3rd step obtained changes, micro-to methoxybenzene and gold nano
Grain mix homogeneously, adds in the diphenyl methane 62.162 parts that mass concentration is 253.386ppm, and stream adds to the esterification of the 1st step
In vertical response still, flow acceleration is 886.146mL/min；Starting esterification vertical response still blender, setting speed is
67.821rpm；Stir 8.9370 minutes；Adding dimercaptosuccinic acid 53.327 parts, it is double that startup is esterified in vertical response still
Level heater, is warming up to 94.679 DEG C, and pH is adjusted between 8.9386, and being passed through chlorine ventilation is 53.825m3/ min, protects
Gentle and quiet put 77.615 minutes；Being again started up being esterified vertical response still blender, rotating speed is 67.526rpm, adds 2,6-diisopropyl
Base phenylisocyanate 47.16 parts so that it is the hydrophilic/hydrophobic single threshold of reactant liquor is 10.97359, and pH is adjusted to
Between 8.9679, insulation stands 86.790 minutes；
5th step: starting the blender in esterification vertical response still, setting speed is 86.23rpm, vertical to esterification while stirring
Reactor adds 2-benzotrifluoride-4-methyl-5-thiazole formic acid ethyl ester 62.835 parts, startup are esterified in vertical response still
Double-stage heating device, sets the temperature in esterification vertical response still as 9.195 × 102DEG C, after being incubated 86.790 minutes, add first
Base-1H-benzimidazolyl-2 radicals-base-carbamate 73.610 parts, carries out enzyme catalysis fluorescentization and reacts 24.690 minutes；Add afterwards
Enter 286.0ppm to chloro-alpha-brominated phenylacetic acid 106.355 parts, start the double-stage heating device in esterification vertical response still, if
Surely the temperature in esterification vertical response still is 153.195 DEG C, and pH adjusts between 8.9825, and pressure is 0.2830MPa, during reaction
Between be 0.937 hour；It is depressurized to 0MPa afterwards, is cooled to 59.19386 DEG C of dischargings, i.e. obtain a kind of rare cultural relics, literature and history shelves
Case, calligraphy and painting protecting agent.
The particle diameter of wherein said gold nano particulate is 37.307 μm.
In the application, described a kind of rare cultural relics, literature and history archives, calligraphy and painting protecting agent needs coordinate with inert diluent makes
With, a kind of rare cultural relics, literature and history archives, calligraphy and painting protecting agent and inert diluent fit quality ratio for 1:888.484；Described inertia
Diluent is: binary copolymerization chlorine ether, and described inert diluent binary copolymerization chlorine ether is common commercial goods.
Embodiment 3
A kind of rare cultural relics, literature and history archives, calligraphy and painting protecting agent of the present invention is prepared according to following steps, and by weight:
1st step: in esterification vertical response still, add and remove silicate cement 228.9562 parts, fatty acyl monoethanolamine polyoxyethylene
20.9605 parts of ether, starts the blender in esterification vertical response still, and setting speed is 21.9849rpm, starts esterification vertical instead
Answer the double-stage heating device in still, make temperature rise to 36.9586 DEG C, add methyl nadic anhydride 23.9504 parts
Stir, carry out enzyme catalysis fluorescentization and react 13.9136 minutes, add N-methyl-N-nitro-p-toluenesulfonamide
19.9511 parts, being passed through flow is 12.9332m3The chlorine of/min 0.921 hour；4-is added afterwards in esterification vertical response still
Nitrophthalimide 22.9596 parts, is again started up the double-stage heating device being esterified in vertical response still, makes temperature rise to
53.9586 DEG C, it is incubated 13.9332 minutes, adds 1-amino-2-methyl anthraquinone 25.9794 parts, adjust in esterification vertical response still
The pH value of solution is 4.89746, is incubated 13.9332 minutes；
2nd step: another depletion nanoparticle 27.952 parts, by gold nano particulate ultrasonic Treatment under power is 5.5391KW
0.919 hour, attrition grinding, and by 408.9748 eye mesh screens；Gold nano particulate is joined another esterification vertical response
In still, add the diphenyl methane 20.9415 parts that mass concentration is 23.9986ppm, disperse gold nano particulate, start esterification vertical
Double-stage heating device in formula reactor, makes solution temperature between 4.89332 × 10 DEG C, starts in esterification vertical response still
Blender, and with 4.89586 × 102Rpm speed stirring, adjust pH value between 4.891, insulated and stirred 5.539 × 10-1Little
Time；Stopped reaction stands 5.539 × 10 minutes afterwards, goes the removal of impurity；Suspension is added 2-to benzotrifluoride-4-methyl-5-
Thiazole ethyl formate 22.9914 parts, adjust pH value between 1.9332, formed precipitate spend silicate cement eluting, by from
Scheming is at rotating speed 4.9748 × 103Solid content is obtained, 2.9386 × 10 under rpm2It is dried at a temperature of DEG C, after grinding, crosses 8.9748
×103Mesh sieve, standby；
3rd step: separately take 4-bromo-1-amino anthraquinones-2-sulfonic acid 22.9854 parts, methoxybenzene 19.9713 parts and the 2nd step are processed
Rear gold nano particulate 27.952 parts, uses X to penetrate top dorsad and penetrates irradiation after mix homogeneously, X penetrates top dorsad and penetrates the energy of irradiation and is
10.9358MeV, dosage are 58.9937kGy, irradiation time is 22.9438 minutes, obtain the 4-bromo-1-amino anthracene that character changes
Quinone-2-sulfonic acid, to methoxybenzene and gold nano particulate mixture；By bromo-for 4-1-amino anthraquinones-2-sulfonic acid, to methoxybenzene and
Gold nano particulate mixture is placed in another esterification vertical response still, starts the double-stage heating device in esterification vertical response still,
Design temperature 21.9746 DEG C, starts the blender in esterification vertical response still, and rotating speed is that 13.9332rpm, pH are adjusted to
Between 4.89358, it is dehydrated 22.9706 minutes, standby；
4th step: 4-bromo-1-amino anthraquinones-2-sulfonic acid that the character that the 3rd step obtained changes, micro-to methoxybenzene and gold nano
Grain mix homogeneously, adds in the diphenyl methane 20.9415 parts that mass concentration is 23.9986ppm, and stream adds to the ester of the 1st step
Changing in vertical response still, flow acceleration is 158.9310mL/min；Starting esterification vertical response still blender, setting speed is
27.9844rpm；Stir 4.89849 minutes；Add dimercaptosuccinic acid 10.9524 parts, start in esterification vertical response still
Double-stage heating device, is warming up to 57.917 DEG C, and pH is adjusted between 4.89986, and being passed through chlorine ventilation is 12.9849m3/
Min, insulation stands 47.9268 minutes；Being again started up being esterified vertical response still blender, rotating speed is 22.9710rpm, adds 2,
6-diisopropyl phenylisocyanate 11.9359 parts so that it is the hydrophilic/hydrophobic single threshold of reactant liquor is 5.5391, and pH is adjusted
Whole between 4.8917, insulation stands 46.9680 minutes；
5th step: starting the blender in esterification vertical response still, setting speed is 19.9521rpm, vertical to esterification while stirring
Formula reactor adds 2-to benzotrifluoride-4-methyl-5-thiazole formic acid ethyl ester 22.9914 parts, startup esterification vertical response still
In double-stage heating device, set esterification vertical response still in temperature as 4.9780 × 102DEG C, after being incubated 46.9680 minutes,
Add methyl isophthalic acid H-benzimidazolyl-2 radicals-base-carbamate 29.9433 parts, carry out enzyme catalysis fluorescentization and react 13.9136 points
Clock；Add afterwards 19.9967ppm to chloro-alpha-brominated phenylacetic acid 52.9296 parts, start the twin-stage in esterification vertical response still
Heater, set esterification vertical response still in temperature as 97.9780 DEG C, pH adjusts between 4.89849, and pressure is
0.199230MPa, the response time is 0.4912 hour；It is depressurized to 0MPa afterwards, is cooled to 54.19917 DEG C of dischargings, i.e. obtains one
Plant rare cultural relics, literature and history archives, calligraphy and painting protecting agent.
The particle diameter of wherein said gold nano particulate is 27.927 μm.
In the application, described a kind of rare cultural relics, literature and history archives, calligraphy and painting protecting agent needs coordinate with inert diluent makes
With, a kind of rare cultural relics, literature and history archives, calligraphy and painting protecting agent and inert diluent fit quality ratio for 1:448.9222；Described lazy
Property diluent is: 4-[4-[[3-[(ethylphenyl amino) sulfonyl]-4-aminomethyl phenyl] azo]-4,5-dihydro-3-methyl-
5-oxygen-1H-pyrazol-1-yl] benzenesulfonic acid, described inert diluent 4-[4-[[3-[(ethylphenyl amino) sulfonyl]-4-methyl
Phenyl] azo]-4,5-dihydro-3-methyl-5-oxygen-1H-pyrazol-1-yl] benzenesulfonic acid is common commercial goods.
Reference examples
Reference examples uses the Collectors Edition archives of certain brand commercially available, valuable information protection agent to carry out archives, books and reference materials Protection.
Embodiment 4
By embodiment 1～3 and reference examples obtained Collectors Edition archives, valuable information protection agent carries out archives, books and reference materials are protected
Protect test, wherein Collectors Edition archives, valuable information protection agent and inert diluent with the use of, Collectors Edition archives, valuable data
Protective agent is 1:448.222 with the mass ratio of inert diluent, and described inert diluent is 5-amino-2-[2-in embodiment 1
[4-(4,5-dihydro-3-methyl-5-oxo-1H-pyrazol-1-yl)-2-sulfophenyl] vinyl]-benzenesulfonic acid, in example 2
For 4-[4-[[3-[(ethylphenyl amino) sulfonyl]-4-aminomethyl phenyl] azo]-4,5-dihydro-3-methyl-5-oxygen-1H-pyrrole
Azoles-1-base] benzenesulfonic acid, it is binary copolymerization chlorine ether in embodiment 3, process variability mould to document after terminating, 10 years documents are intact
The parameters such as rate, protective rate, document clean surface ratio are analyzed.Process data are as shown in table 1.
As seen from Table 1, a kind of rare cultural relics, literature and history archives, calligraphy and painting protecting agent of the present invention, the mould variability of its document,
The parameters such as 10 years document serviceability rates, protective rate, document clean surface ratios are above the product that prior art produces.
Additionally, as shown in Figures 1 to 3, it is that a kind of rare cultural relics, literature and history archives, calligraphy and painting protecting agent of the present invention are with right
Carried out as usual, with the time of use change test data statistics.Figure is found out, embodiment 1～3 harmful organism fatality rate,
Protective agent coefficient of stabilization, use after the technical specification such as document regeneration rate, be the most significantly better than the product that prior art produces.
Claims (7)
1. rare cultural relics, literature and history archives, calligraphy and painting protecting agent, it is characterised in that by following components proportioning group by weight
Become: remove silicate cement 228.562～453.27 parts, fatty acyl monoethanolamine polyoxyethylene ether 20.605～62.307 parts, methyl
Tetrahydrophthalic anhydride 23.504～132.222 parts, N-methyl-N-nitro-p-toluenesulfonamide 19.511～36.484
Part, 4-nitrophthalimide 22.596～79.47 parts, 1-amino-2-methyl anthraquinone 25.794～86.228 parts, 4-
Bromo-1-amino anthraquinones-2-sulfonic acid 22.854～45.148 parts, to methoxybenzene 19.713～64.715 parts, gold nano particulate
27.52～82.476 parts, diphenyl methane 20.415～62.162 parts, dimercaptosuccinic acid 10.524～53.327 parts, 2,6-
Diisopropyl phenylisocyanate 11.359～47.16 parts, 2-to benzotrifluoride-4-methyl-5-thiazole formic acid ethyl ester 22.914～
62.835 parts, methyl isophthalic acid H-benzimidazolyl-2 radicals-base-carbamate 29.433～73.610 parts, mass concentration is 19.967ppm
～286.0ppm to chloro-alpha-brominated phenylacetic acid 52.296～106.355 parts.
A kind of rare cultural relics, literature and history archives, calligraphy and painting protecting agent the most according to claim 1, it is characterised in that by following group
Point by weight proportioning composition: remove silicate cement 229.562～452.27 parts, fatty acyl monoethanolamine polyoxyethylene ether
21.605～61.307 parts, methyl nadic anhydride 24.504～131.222 parts, N-methyl-N-nitroso is to first
Benzsulfamide 20.511～35.484 parts, 4-nitrophthalimide 23.596～78.47 parts, 1-amino-2-methyl anthracene
Quinone 26.794～85.228 parts, 4-bromo-1-amino anthraquinones-2-sulfonic acid 23.854～44.148 parts, to methoxybenzene 20.713～
63.715 parts, gold nano particulate 28.52～81.476 parts, diphenyl methane 21.415～61.162 parts, dimercaptosuccinic acid
11.524～52.327 parts, 2,6-diisopropyl phenylisocyanates 12.359～46.16 parts, 2-is to benzotrifluoride-4-methyl-5-
Thiazole ethyl formate 23.914～61.835 parts, methyl isophthalic acid H-benzimidazolyl-2 radicals-base-carbamate 30.433～72.610
Part, mass concentration be 20.967ppm～285.0ppm to chloro-alpha-brominated phenylacetic acid 53.296～105.355 parts.
A kind of rare cultural relics the most according to claim 1 and 2, literature and history archives, the preparation method of calligraphy and painting protecting agent, its feature
It is, by weight, comprises the steps:
1st step: in esterification vertical response still, add and remove silicate cement and fatty acyl monoethanolamine polyoxyethylene ether, start ester
Changing the blender in vertical response still, setting speed is 21.849rpm～67.706rpm, starts in esterification vertical response still
Double-stage heating device, makes temperature rise to 36.586 DEG C～37.420 DEG C, adds methyl nadic anhydride and stirs,
Carry out enzyme catalysis fluorescentization to react 13.136～24.825 minutes, add N-methyl-N-nitro-p-toluenesulfonamide, be passed through stream
Amount is 12.332m3/ min～53.690m3The chlorine 0.21 of/min～0.86 hour；Add in esterification vertical response still afterwards
4-nitrophthalimide, is again started up the double-stage heating device being esterified in vertical response still, makes temperature rise to 53.586
DEG C～86.420 DEG C, be incubated 13.332～24.359 minutes, add 1-amino-2-methyl anthraquinone, adjust esterification vertical response still
The pH value of middle solution is 4.8746～8.9962, is incubated 13.332～253.359 minutes；
2nd step: another depletion nanoparticle, by gold nano particulate ultrasonic Treatment under power is 5.531KW～10.97359KW
0.19～0.86 hour, attrition grinding, and by 408.748～508.980 eye mesh screens；Gold nano particulate is joined another
In esterification vertical response still, add the diphenyl methane dispersion gold nano that mass concentration is 23.986ppm～253.386ppm micro-
Grain, starts the double-stage heating device in esterification vertical response still, makes solution temperature at 4.8332 × 10 DEG C～8.9420 × 10 DEG C
Between, start the blender in esterification vertical response still, and with 4.8586 × 102Rpm～8.9706 × 102The speed of rpm is stirred
Mix, adjust pH value between 4.81～8.9359, insulated and stirred 5.53 × 10-1～10.97 × 10-1Hour；Stopped reaction afterwards
Stand 5.53 × 10～10.97 × 10 minutes, go the removal of impurity；Suspension is added 2-to benzotrifluoride-4-methyl-5-thiazole first
Acetoacetic ester, adjustment pH value, between 1.332～2.690, forms precipitate and spends silicate cement eluting, by centrifuge at rotating speed
4.748×103Rpm～9.980 × 103Solid content is obtained, 2.386 × 10 under rpm2DEG C～3.706 × 102Do at a temperature of DEG C
Dry, cross 8.748 × 10 after grinding3～9.980 × 103Mesh sieve, standby；
3rd step: separately take 4-bromo-1-amino anthraquinones-2-sulfonic acid, methoxybenzene and the 2nd step are processed after gold nano particulate, mixing is all
Use X to penetrate top dorsad after even and penetrate irradiation, X penetrate top dorsad penetrate the energy of irradiation be 10.358MeV～38.370MeV, dosage be
58.937kGy～98.624kGy, irradiation time are 22.438～47.541 minutes, obtain the 4-bromo-1-amino anthracene that character changes
Quinone-2-sulfonic acid, to methoxybenzene and gold nano particulate mixture；By bromo-for 4-1-amino anthraquinones-2-sulfonic acid, to methoxybenzene and
Gold nano particulate mixture is placed in another esterification vertical response still, starts the double-stage heating device in esterification vertical response still,
Design temperature 21.746 DEG C～67.690 DEG C, start esterification vertical response still in blender, rotating speed be 13.332rpm～
408.1rpm, pH are adjusted between 4.8358～8.9370, are dehydrated 22.706～36.136 minutes, standby；
4th step: 4-bromo-1-amino anthraquinones-2-sulfonic acid that the character that the 3rd step obtained changes, micro-to methoxybenzene and gold nano
Grain mix homogeneously, adds in the diphenyl methane that mass concentration is 23.986ppm～253.386ppm, and stream adds to the 1st step
In esterification vertical response still, flow acceleration is 158.310mL/min～886.146mL/min；Start esterification vertical response still to stir
Mixing machine, setting speed is 27.844rpm～67.821rpm；Stir 4.8849～8.9370 minutes；Add dimercapto succinum
Acid, starts the double-stage heating device in esterification vertical response still, is warming up to 57.17 DEG C～94.679 DEG C, and pH is adjusted to 4.8986
～between 8.9386, being passed through chlorine ventilation is 12.849m3/ min～53.825m3/ min, insulation stands 47.268～77.615
Minute；Being again started up being esterified vertical response still blender, rotating speed is 22.710rpm～67.526rpm, adds 2,6-diisopropyl
Phenylisocyanate so that it is the hydrophilic/hydrophobic single threshold of reactant liquor is 5.531～10.97359, and make pH be adjusted to 4.817～
Between 8.9679, insulation stands 46.680～86.790 minutes；
5th step: starting the blender in esterification vertical response still, setting speed is 19.521rpm～86.23rpm, while stirring
In esterification vertical response still, add 2-benzotrifluoride-4-methyl-5-thiazole formic acid ethyl ester, startup are esterified in vertical response still
Double-stage heating device, set esterification vertical response still in temperature as 4.780 × 102DEG C～9.195 × 102DEG C, insulation
After 46.680～86.790 minutes, adding methyl isophthalic acid H-benzimidazolyl-2 radicals-base-carbamate, enzyme catalysis fluorescentization is reacted
13.136～24.690 minutes；Add afterwards chloro-alpha-brominated phenylacetic acid, start the double-stage heating dress in esterification vertical response still
Put, set esterification vertical response still in temperature as 97.780 DEG C～153.195 DEG C, pH adjust to 4.8849～8.9825 it
Between, pressure is 0.19230MPa～0.2830MPa, and the response time is 0.412～0.937 hour；It is depressurized to 0MPa afterwards, cooling
To 54.1917 DEG C～59.19386 DEG C of dischargings, i.e. obtain a kind of rare cultural relics, literature and history archives, calligraphy and painting protecting agent.
A kind of rare cultural relics the most according to claim 3, literature and history archives, the preparation method of calligraphy and painting protecting agent, its feature exists
In, the particle diameter of described gold nano particulate is 27.27 μm～37.307 μm.
A kind of rare cultural relics the most according to claim 1, literature and history archives, calligraphy and painting protecting agent are mainly used in for containing figure
Book, document protection process in application.
Application the most according to claim 5, it is characterised in that described books, document are sudd document, mud plate document, sheep
Skin document, the inscriptions on bones or tortoise shells are offered, inscription on ancient bronze objects document, letter wooden tablets or slips for writing document, stone inscription document, fine silk silks document, ancient character draw at least one.
Application the most according to claim 5, it is characterised in that described a kind of rare cultural relics, literature and history archives, calligraphy and painting protecting agent
With inert diluent with the use of, a kind of rare cultural relics, literature and history archives, calligraphy and painting protecting agent with inert diluent fit quality ratio are
1:448.222～888.484；Described inert diluent is: 1. 5-amino-2-[2-[4-(4,5-dihydro-3-methyl-5-oxo-
1H-pyrazol-1-yl)-2-sulfophenyl] vinyl]-benzenesulfonic acid, 2. 4-[4-[[3-[(ethylphenyl amino) sulfonyl]-4-first
Base phenyl] azo]-4,5-dihydro-3-methyl-5-oxygen-1H-pyrazol-1-yl] in benzenesulfonic acid, 3. three kinds of binary copolymerization chlorine ether
One, described inert diluent is common commercial goods.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106824265A (en) * | 2016-12-26 | 2017-06-13 | 徐州工程学院 | Spray aerogel drop haze cold clouds and preparation method thereof in a kind of high-altitude |
| CN112048049A (en) * | 2019-06-06 | 2020-12-08 | 中国科学院化学研究所 | Luminescent polymer and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102450250A (en) * | 2010-10-20 | 2012-05-16 | 周端午 | Bacteriostatic mildew-resistant insecticidal sustained release agent prepared from sol/gel also used as insect attractant |
| CN105713744A (en) * | 2016-01-26 | 2016-06-29 | 孟根森 | Cleaning and treating agent for textile fabrics |
-
2016
- 2016-07-11 CN CN201610543239.2A patent/CN106172492A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102450250A (en) * | 2010-10-20 | 2012-05-16 | 周端午 | Bacteriostatic mildew-resistant insecticidal sustained release agent prepared from sol/gel also used as insect attractant |
| CN105713744A (en) * | 2016-01-26 | 2016-06-29 | 孟根森 | Cleaning and treating agent for textile fabrics |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106824265A (en) * | 2016-12-26 | 2017-06-13 | 徐州工程学院 | Spray aerogel drop haze cold clouds and preparation method thereof in a kind of high-altitude |
| CN112048049A (en) * | 2019-06-06 | 2020-12-08 | 中国科学院化学研究所 | Luminescent polymer and preparation method and application thereof |
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Application publication date: 20161207 |