CN107856156B - A kind of preparation method of nm TiO 2-base timber preservative - Google Patents
A kind of preparation method of nm TiO 2-base timber preservative Download PDFInfo
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- CN107856156B CN107856156B CN201711166311.5A CN201711166311A CN107856156B CN 107856156 B CN107856156 B CN 107856156B CN 201711166311 A CN201711166311 A CN 201711166311A CN 107856156 B CN107856156 B CN 107856156B
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- tio
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- timber preservative
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
- B27K3/00—Impregnating wood, e.g. impregnation pretreatment, for example puncturing; Wood impregnation aids not directly involved in the impregnation process
- B27K3/52—Impregnating agents containing mixtures of inorganic and organic compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/14—Methyl esters, e.g. methyl (meth)acrylate
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
- B27K2240/00—Purpose of the treatment
- B27K2240/20—Removing fungi, molds or insects
Abstract
A kind of nm TiO 2-base timber preservative, it is characterized in that, it includes, the modification of nano-titanium dioxide, the preparation of acrylic emulsion, acrylic acid aqueous dispersions are uniformly mixed with Tebuconazole, carbendazim, imidacloprid, obtain nm TiO 2-base timber preservative by the preparation of acrylic acid aqueous dispersions.Timber preservative provided by the invention has broad-spectrum sterilization and insecticidal action, favorable anti-corrosion effect, while toxicity is smaller, non-hazardous to environment and human body.
Description
Technical field
The present invention relates to a kind of timber preservative, especially a kind of preparation side of nm TiO 2-base timber preservative
Method.
Background technique
Using the small-size effect of nano material, quantum effect, interface or skin effect, can obtain with multiple performance
Nano preservative, Antimicrobial preservative, resistance to phototropic, resistant to heat aging Multifucntional timber preservative can be prepared.Nano wood
Material preservative makes it that can become new with excellent properties such as the controllabilitys of its good permeability, resistance leachability and effective component
The timber preservative of a generation also results in the special attention of domestic and international researcher.
The nano-TiO of high security2With the efficient functions such as harmful bacteria, degradable organic pollutant are killed, it not only can
Sterilization can also be such that the endotoxin generated after bacterial fungus is dead decomposes.But nano-TiO2The large specific surface area of particle,
By the effect of Van der Waals force in liquid phase medium, easily reunite, to form larger-size aggregate, it can be seriously affected
Practical application effect.Therefore, nano-TiO is improved2Dispersibility in water is to prepare nano-TiO2The key of preservative.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of the nm TiO 2-base timber preservative of good dispersion.
To achieve the goals above, present invention employs following technical solutions:
A kind of nm TiO 2-base timber preservative, which is characterized in that it includes the modification of nano-titanium dioxide, and third
The preparation of olefin(e) acid lotion, the preparation of acrylic acid aqueous dispersions mix acrylic acid aqueous dispersions and Tebuconazole, carbendazim, imidacloprid
It closes uniformly, obtains nm TiO 2-base timber preservative.
The nm TiO 2-base timber preservative, which is characterized in that it, which has the following steps, is prepared:
(1) nano-titanium dioxide and DMF are added in reaction vessel, titanate esters NDZ-105, regulated value to 7.5- is added
8, magnetic agitation 30-40min are added isophorone diisocyanate, are transferred in 80-85 DEG C of water-bath, temperature constant magnetic stirring
6-8h is reacted, reduces temperature to room temperature, filtering is washed 2-3 times using methylene chloride, is placed in 35-40 DEG C of vacuum oven and is done
It is dry, obtain modified nano-titanium dioxide；
(2) acrylic acid, methyl methacrylate, Methacrylamide are mixed with the mass ratio of 1:3-4:0.2-0.3 and is stirred
It mixes uniformly, obtains mix monomer；By OP-10, dodecyl sodium sulfate and deionized water with the mass ratio of 1:1.2-1.5:25-30
It is mixed evenly, adds the NaHCO of 2-2.2 times of parts by weight3, continues to mix and stir evenly, obtain emulsion；
(3) emulsion and 1/ of propylene glycol methyl ether acetate, 1/2 is added in the reaction kettle equipped with condenser pipe and blender
1/2 sodium peroxydisulfate solution is added after mixing evenly in 5 mix monomer, is warming up to 75-85 DEG C, temperature constant magnetic stirring 50-
60min obtains pre-polymerization lotion；Remaining mix monomer and emulsion are added dropwise simultaneously, control is dripped off in 1.5-2h, during which divides 5-6
Secondary that remaining sodium peroxydisulfate solution is added, then 75-85 DEG C of heat preservation magnetic agitation 4-6h, reduces temperature to 30 DEG C, with ammonium hydroxide tune
Section system pH obtains acrylic emulsion with the screen filtration of 80-100 mesh for 7-8；
(4) acrylic emulsion is mixed with deionized water with the mass ratio of 1:1-1.5, after mechanical stirring is uniform, addition changes
Property nano-titanium dioxide, moistening flatting agent MONENG-1154 and organic silicon defoamer, stir, obtain propylene sour water
Dispersion liquid；Tebuconazole, carbendazim and imidacloprid are added in propylene glycol phenyl ether, is stirred well to uniformly, adds it to
In acrylic acid aqueous dispersions, continues magnetic agitation 50-60min, obtain nm TiO 2-base timber preservative.
The preparation method of the nm TiO 2-base timber preservative, which is characterized in that nano-silica in step (1)
The mass ratio for changing titanium, DMF, titanate esters NDZ-105 and isophorone diisocyanate is 1:60-70:0.08-0.1:0.05-
0.06。
The preparation method of the nm TiO 2-base timber preservative, which is characterized in that mix monomer in step (2)
It is ready-to-use with emulsion.
The preparation method of the nm TiO 2-base timber preservative, which is characterized in that propylene glycol first in step (3)
Ether acetate, emulsion, mix monomer and sodium peroxydisulfate solution mass ratio be 1:10-12:6-8:1.2-1.5.
The preparation method of the nm TiO 2-base timber preservative, which is characterized in that sodium peroxydisulfate in step (3)
The concentration of solution is 0.01-0.012mol/L, the ammonium hydroxide that ammonium hydroxide is 10%.
The preparation method of the nm TiO 2-base timber preservative, which is characterized in that propylene yogurt in step (4)
Liquid, modified nano-titanium dioxide, moistening flatting agent MONENG-1154, organic silicon defoamer mass ratio be 1:0.06-0.08:
0.01-0.02:0.02-0.03.
The preparation method of the nm TiO 2-base timber preservative, which is characterized in that propylene glycol phenyl in step (4)
Base ether, Tebuconazole, carbendazim, imidacloprid, acrylic acid aqueous dispersions mass ratio be 1:0.03-0.04:0.02-0.03:
0.012-0.015:4-5.
By using above-mentioned technical solution, the invention has the following beneficial effects:
Titanate esters NDZ-105 of the present invention and isophorone diisocyanate carry out modification, titanium to nano-titanium dioxide
Acid esters NDZ-105 can soak nano grain surface, reduce its surface energy, it is special to maintain nano-titanium dioxide anatase crystalline structure
Sign, preferably keeps its photocatalysis performance；And isophorone diisocyanate can be reacted with acrylic acid, further increase nanometer
Degree of scatter of the titanium dioxide in acrylic emulsion.It also added Tebuconazole, carbendazim, pyrrole in timber preservative of the invention
Worm quinoline, can inhibit the synthesis of ergosterol, the development of interference fungi attachment spore and haustorium, influence growth and the spore of mycelia
It is formed, enhances it and power is resisted to termite etc., have the characteristics that efficient, wide sterilization spectrum, strong absorbability, less toxic to people and animals.This hair
The timber preservative of bright offer has broad-spectrum sterilization and insecticidal action, favorable anti-corrosion effect, while toxicity is smaller, to environment and people
Body is non-hazardous.
Specific embodiment
The nm TiO 2-base timber preservative of the present embodiment, has the following steps and is prepared:
(1) nano-titanium dioxide and DMF are added in reaction vessel, addition titanate esters NDZ-105, regulated value to 7.5,
Magnetic agitation 40min is added isophorone diisocyanate, is transferred in 85 DEG C of water-baths, and temperature constant magnetic stirring reacts 8h, drop
Low temperature to room temperature, filtering is washed 3 times using methylene chloride, is placed in drying in 40 DEG C of vacuum ovens, is obtained modified Nano two
Titanium oxide；
(2) acrylic acid, methyl methacrylate, Methacrylamide are mixed evenly with the mass ratio of 1:4:0.2,
Obtain mix monomer；OP-10, dodecyl sodium sulfate and deionized water are mixed evenly with the mass ratio of 1:1.2:30,
Add the NaHCO of 2 times of parts by weight3, continues to mix and stir evenly, obtain emulsion；
(3) emulsion and 1/ of propylene glycol methyl ether acetate, 1/2 is added in the reaction kettle equipped with condenser pipe and blender
1/2 sodium peroxydisulfate solution is added after mixing evenly in 5 mix monomer, is warming up to 85 DEG C, and temperature constant magnetic stirring 60min is obtained
To pre-polymerization lotion；Remaining mix monomer and emulsion are added dropwise simultaneously, control drips off in 2h, during which divides 6 times and remaining mistake is added
Metabisulfite solution, then 85 DEG C of heat preservation magnetic agitation 6h, reduce temperature to 30 DEG C, are 8 with ammonia water conditioning system pH value, with 100
Purpose screen filtration, obtains acrylic emulsion；
(4) acrylic emulsion is mixed with deionized water with the mass ratio of 1:1.5, after mechanical stirring is uniform, is added and is modified
Nano-titanium dioxide, moistening flatting agent MONENG-1154 and organic silicon defoamer, stir, and obtain acrylic acid moisture
Dispersion liquid；Tebuconazole, carbendazim and imidacloprid are added in propylene glycol phenyl ether, is stirred well to uniformly, adds it to third
In olefin(e) acid aqueous dispersions, continues magnetic agitation 60min, obtain nm TiO 2-base timber preservative.
Nano-titanium dioxide in step (1), DMF, titanate esters NDZ-105 and isophorone diisocyanate mass ratio be
1:70:0.08:0.06.
Mix monomer and emulsion are ready-to-use in step (2).
Propylene glycol methyl ether acetate in step (3), emulsion, mix monomer and sodium peroxydisulfate solution mass ratio be 1:
12:8:1.5.
The concentration of sodium peroxydisulfate solution is 0.01mol/L, the ammonium hydroxide that ammonium hydroxide is 10% in step (3).
Acrylic emulsion, modified nano-titanium dioxide, moistening flatting agent MONENG-1154, organosilicon defoaming in step (4)
The mass ratio of agent is 1:0.08:0.01:0.02.
Propylene glycol phenyl ether in step (4), Tebuconazole, carbendazim, imidacloprid, acrylic acid aqueous dispersions mass ratio be 1:
0.03:0.02:0.012:5.
Claims (7)
1. a kind of preparation method of nm TiO 2-base timber preservative, which is characterized in that it includes, nano-titanium dioxide
It is modified, the preparation of acrylic emulsion, the preparation of acrylic acid aqueous dispersions, by acrylic acid aqueous dispersions and Tebuconazole, carbendazim, pyrrole
Worm quinoline is uniformly mixed, and obtains nm TiO 2-base timber preservative；
It is specific the preparation method comprises the following steps:
(1) nano-titanium dioxide and DMF are added in reaction vessel, titanate esters NDZ-105, regulated value to 7.5-8, magnetic is added
Power stirs 30-40min, and isophorone diisocyanate is added, is transferred in 80-85 DEG C of water-bath, temperature constant magnetic stirring reaction
6-8h reduces temperature to room temperature, and filtering is washed 2-3 times using methylene chloride, is placed in drying in 35-40 DEG C of vacuum oven, is obtained
To modified nano-titanium dioxide；
(2) acrylic acid, methyl methacrylate, Methacrylamide are mixed with the mass ratio of 1:3-4:0.2-0.3 equal
It is even, obtain mix monomer；OP-10, dodecyl sodium sulfate and deionized water are mixed with the mass ratio of 1:1.2-1.5:25-30
It stirs evenly, adds the NaHCO of 2-2.2 times of parts by weight3, continues to mix and stir evenly, obtain emulsion；
(3) emulsion and 1/5 of propylene glycol methyl ether acetate, 1/2 is added in the reaction kettle equipped with condenser pipe and blender
1/2 sodium peroxydisulfate solution is added after mixing evenly in mix monomer, is warming up to 75-85 DEG C, temperature constant magnetic stirring 50-60min,
Obtain pre-polymerization lotion；Remaining mix monomer and emulsion are added dropwise simultaneously, control is dripped off in 1.5-2h, during which divides 5-6 addition
Remaining sodium peroxydisulfate solution, then 75-85 DEG C of heat preservation magnetic agitation 4-6h, reduces temperature to 30 DEG C, uses ammonia water conditioning system
PH value is 7-8, with the screen filtration of 80-100 mesh, obtains acrylic emulsion；
(4) acrylic emulsion is mixed with deionized water with the mass ratio of 1:1-1.5, after mechanical stirring is uniform, modification is added and receives
Rice titanium dioxide, moistening flatting agent MONENG-1154 and organic silicon defoamer, stir, obtain acrylic acid water dispersion
Liquid；Tebuconazole, carbendazim and imidacloprid are added in propylene glycol phenyl ether, is stirred well to uniformly, adds it to propylene
In sour water dispersion liquid, continues magnetic agitation 50-60min, obtain nm TiO 2-base timber preservative.
2. the preparation method of nm TiO 2-base timber preservative according to claim 1, which is characterized in that step
(1) nano-titanium dioxide in, DMF, titanate esters NDZ-105 and isophorone diisocyanate mass ratio be 1:60-70:
0.08-0.1:0.05-0.06.
3. the preparation method of nm TiO 2-base timber preservative according to claim 1, which is characterized in that step
(2) mix monomer and emulsion are ready-to-use in.
4. the preparation method of nm TiO 2-base timber preservative according to claim 1, which is characterized in that step
(3) propylene glycol methyl ether acetate in, emulsion, mix monomer and sodium peroxydisulfate solution mass ratio be 1:10-12:6-8:1.2-
1.5。
5. the preparation method of nm TiO 2-base timber preservative according to claim 1, which is characterized in that step
(3) concentration of sodium peroxydisulfate solution is 0.01-0.012mol/L, the ammonium hydroxide that ammonium hydroxide is 10% in.
6. the preparation method of nm TiO 2-base timber preservative according to claim 1, which is characterized in that step
(4) acrylic emulsion in, modified nano-titanium dioxide, moistening flatting agent MONENG-1154, organic silicon defoamer mass ratio be
1:0.06-0.08:0.01-0.02:0.02-0.03.
7. the preparation method of nm TiO 2-base timber preservative according to claim 1, which is characterized in that step
(4) propylene glycol phenyl ether in, Tebuconazole, carbendazim, imidacloprid, acrylic acid aqueous dispersions mass ratio be 1:0.03-0.04:
0.02-0.03:0.012-0.015:4-5.
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| CN107856156B true CN107856156B (en) | 2019-05-03 |
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| WO2005114078A2 (en) * | 2004-05-13 | 2005-12-01 | Osmose, Inc. | Compositions and methods for treating cellulose-based materials with micronized additives |
| CN102009037B (en) * | 2010-10-25 | 2013-06-19 | 江苏考普乐新材料股份有限公司 | Method for protecting metal by photoelectrochemistry |
| CN104744972B (en) * | 2013-12-25 | 2017-06-09 | 江苏考普乐新材料有限公司 | Modified Alumina gel and ceramic coating and preparation method thereof |
| CN104859010A (en) * | 2014-12-25 | 2015-08-26 | 王玉燕 | Nano titanium dioxide modified wood production method |
| CN104927515A (en) * | 2015-05-27 | 2015-09-23 | 芜湖县双宝建材有限公司 | Waterproof high-adhesive-force corrosion-resistant coating for ships |
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Granted publication date: 20190503 Termination date: 20191121 |