CN107932668A - The preparation method of aqueous wood preservative is lost in a kind of anti-current - Google Patents
The preparation method of aqueous wood preservative is lost in a kind of anti-current Download PDFInfo
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- CN107932668A CN107932668A CN201711114461.1A CN201711114461A CN107932668A CN 107932668 A CN107932668 A CN 107932668A CN 201711114461 A CN201711114461 A CN 201711114461A CN 107932668 A CN107932668 A CN 107932668A
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- rosin
- granatum
- lost
- preparation
- wood 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
-
- 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
The present invention relates to the preparation method that aqueous wood preservative is lost in a kind of anti-current, belong to wood preservation technical field.Rosin magma is made in the present invention first from rosin, the extracting solution rich in tannin and protein is obtained from granatum and soybean, by rosin magma and extracting solution blending and and acid reaction, play anti-corrosion and filling effect, improve the preservation of timber against decay, the tannin and proteinaceous components added in aqueous wood preservative can establish a polymer network in wood, borate family compound is anchored in processing material, improve the leach resistance of preservative, rosin magma with positive charge, it can play the role of protecting borate, rosin magma has hydrophobicity, the wettability power of timber can be reduced, water content in timber can not meet the microbe survivals such as domestomycetes, moisture condition necessary to procreation, so as to improve the corrosion resistant ability of timber, have broad application prospects.
Description
Technical field
The present invention relates to the preparation method that aqueous wood preservative is lost in a kind of anti-current, belong to wood preservation technical field.
Background technology
Timber is unique reproducible structural material in four big materials, has the spies such as nontoxic, pollution-free, beautiful, easy processing
Point, it is most affine with the mankind, it is the green natural product being favored by people.But the main component of timber is lignin, cellulose
And hemicellulose, it is easily rotten by entomogenous fungi erosion in the case where temperature, moisture, humidity, acid-base value are suitable, cause timber
Service life shortens.How efficiently, timber resources, prolonging wood service life are rationally utilized, it has also become the problem of urgent need to resolve.
According to domestic and international statistics, the service life of the timber after preservative treatment can extend 5~6 times.Therefore, timber is carried out at anti-corrosion
Reason is prolonging wood service life, it is horizontal to improve wood utilization, saves the important channel of timber resources and means.
At present, some timber preservatives of in the market application, such as lindane, penta sodium pentachlorophenate, copper chromium arsenic, due to ring easy to pollute
Border, is progressively disabled or is limited the use of.The borate family compound anti-corrosions such as borax, boric acid, four eight Boratexes of hydration (DOT)
Agent, it is environmental-friendly because having, have no irritating odor, permeability is stronger, to people and animals' low toxicity, to the prevention effect of rot fungi and worm ant
It is good, and timber color and luster in itself and processing performance are not influenced, and when drugloading rate is higher, it is a degree of can also to assign timber
The advantages that anti-flammability and be subject to widely studied and exploitation, borate family compound becomes the more important wood preservation of in the market
Agent.
Although a variety of aqueous wood preservatives such as boric acid class, copper salt kind have domestomycetes very strong inhibitory action,
Antisepsis is faced in use due to easily outflowing with water to decline, endanger the problems such as aqueous bio.How these are strengthened easy
The timber preservative of loss is fixed in wood, is the problem that aqueous wood preservative faces.
Therefore, invent a kind of anti-current mistake type timber preservative has positive meaning to wood preservation technical field.
The content of the invention
The technical problem of major fate of the present invention, it is in use for borate family aqueous wood preservative common at present
Face antisepsis due to easily outflowing with water to decline, endanger the defects of aqueous bio, there is provided aqueous wood is lost in a kind of anti-current
The preparation method of preservative.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
The preparation method of aqueous wood preservative is lost in a kind of anti-current, it is characterised in that specifically preparation process is：
（1）Rosin and isopropanol and sodium hydroxide are loaded and carry thermometer and the four-hole boiling flask of blender and reflux
In, heat temperature raising in water-bath, insulated and stirred are put into, then epoxychloropropane and triethylamine are added into four-hole boiling flask, reflux is anti-
Should after be distilled to recover unreacted epoxychloropropane and triethylamine, obtain self fixing cationic rosin magma；
（2）Weigh granatum and crush 20~30min, obtain granatum crushed material, obtained after granatum crushed material and water are mixed
Mixed liquor, then sodium sulfite is added into mixed liquor, oil bath heating heating, insulation 3~5h of extraction, is separated by filtration to obtain filtrate,
As granatum extracting solution；
（3）Heat temperature raising after soybean and milk and sodium chloride solution are mixed, insulated and stirred extract 40~60min, filtering point
Leave away and remove filter residue, obtain protein extract；
（4）Count in parts by weight, weigh 30~40 portions of self fixing cationic rosin magmas, 10~15 parts of granatum extracting solutions, 8~10 parts
Protein extract is sequentially loaded into the three-necked flask with blender, is started blender and is stirred to obtain prefabricated solution；
（5）Trimethylborate and neopelex are added into the above-mentioned three-necked flask equipped with prefabricated solution, by three mouthfuls of burnings
Bottle is moved into water-bath, heat temperature raising, discharges after 1~2h of stirring reaction, aqueous wood preservative is lost up to anti-current.
Step（1）Described in rosin and the mass ratio of isopropanol and sodium hydroxide be 3:4:1, the temperature of heat temperature raising
For 60~70 DEG C, the insulated and stirred time is 20~30min, and the addition of epoxychloropropane is equal with rosin quality, triethylamine
Addition is the 70~80% of rosin quality, and the temperature of back flow reaction is 75~85 DEG C, and the time of back flow reaction is 18~20h.
Step（2）Described in granatum crushed material and water mass ratio be 1:20, the addition of sodium sulfite is pomegranate
The 0.5~0.8% of cortex amount, the temperature of heat temperature raising is 100~105 DEG C.
Step（3）Described in soybean and the mass ratio of milk and sodium chloride solution be 1:1:3, the matter of sodium chloride solution
It is 50% to measure fraction, and the temperature of heat temperature raising is 50~60 DEG C.
Step（4）Described in the rotating speed being stirred be 200~300r/min, the time being stirred for 20~
30min。
Step（5）Described in trimethylborate addition be prefabricated solution quality 20~30%, dodecyl benzene sulfonic acid
The addition of sodium is the 3~5% of prefabricated solution quality, and the temperature of heat temperature raising is 50~60 DEG C, and the time for stirring reaction is 1~2h.
The beneficial effects of the invention are as follows：
（1）The present invention is first using rosin as raw material, chemically modified obtained self fixing cationic rosin magma, respectively from granatum
The extracting solution rich in tannin and protein is obtained with extraction in soybean, then self fixing cationic rosin magma and extracting solution are blended, with
Trimethylborate reacts, and water base preservative is made in the final anti-current mistake aqueous wood preservative being made containing borate, the present invention
In due to trimethylborate and water reaction generation boric acid, sodium chloride and cationization in the boric acid and protein extract of generation
Excessive boric acid salt component of the sodium hydroxide reaction generation with wood preservation performance in rosin magma, borate companion during use
Water base immersion wood internal, the complete trimethylborate of unreacted continue to continue to generate boric acid with the reaction of moisture in wood cell,
Antisepsis is played, and the borate entered between lumber fibre had not only played antisepsis, but also filling timber gap is played,
Improve the effect of timber consistency so that moisture is difficult to enter wood internal, further improves the preservation of timber against decay；
（2）The tannin and proteinaceous components added in aqueous wood preservative of the present invention can establish a condensate in wood
Network, after the network is fixed, can make with wood components covalent bond or by way of being coagulated together with wood components
For coupling between borate, borate family compound is set to anchor in processing material, so that the turnover rate of boron in processing material is reduced,
The leach resistance of preservative is improved, in addition self fixing cationic rosin magma carries positive charge due to itself, can be carried with surface
The wood-cellulose of negative electrical charge combines, and is voluntarily attached on fiber, and the rosin magma of attachment can play protection borate
Effect, further increase the leach resistance of anti-corrosion active ingredient borate, in addition rosin magma has hydrophobicity, uses
Appropriate rosin processing, can close the free hydroxyl group in timber, so that the wettability power of timber is reduced, simultaneously because reducing
The hygroscopicity of timber, the water content in timber can not meet moisture condition necessary to the microbe survivals such as domestomycetes, procreation, from
And the corrosion resistant ability of timber is improved, have broad application prospects.
Embodiment
It is 3 in mass ratio:4:Rosin and isopropanol and sodium hydroxide are loaded with thermometer and blender and returned by 1
In the four-hole boiling flask for flowing device, it is put into water-bath and is heated to 60~70 DEG C, 20~30min of insulated and stirred, then to four mouthfuls
The epoxychloropropane of quality and the triethylamines of rosin quality 70~80% such as rosin are added in flask, is flowed back at 75~85 DEG C anti-
Unreacted epoxychloropropane and triethylamine are distilled to recover after answering 18~20h, self fixing cationic rosin magma is obtained, weighs granatum
20~30min of crushing in tissue pulverizer is put into, obtains granatum crushed material, is 1 in mass ratio by granatum crushed material and water:
Mixed liquor is obtained after 20 mixing, then the sodium sulfite of granatum quality 0.5~0.8% is added into mixed liquor, oil bath heating heating
To 100~105 DEG C of insulation 3~5h of extraction, be separated by filtration to obtain filtrate, be granatum extracting solution, by soybean and milk and
The sodium chloride solution that mass fraction is 50% is 1 in mass ratio:1:50~60 DEG C are heated to after 3 mixing, insulated and stirred extraction
40~60min, is separated by filtration removal filter residue, obtains protein extract, counts in parts by weight, weighs 30~40 parts of cationization pines
Fragrant magma, 10~15 parts of granatum extracting solutions, 8~10 parts of protein extracts are sequentially loaded into the three-necked flask with blender,
Start blender to be stirred 20~30min with 200~300r/min rotating speeds and obtain prefabricated solution, to it is above-mentioned equipped with prefabricated solution three
The trimethylborate of prefabricated solution quality 20~30% and the neopelex of prefabricated solution quality 3~5% are added in mouth flask,
Three-necked flask is moved into water-bath, 50~60 DEG C is heated to, discharges after 1~2h of stirring reaction, up to anti-current dehydration base
Timber preservative.
Example 1
It is 3 in mass ratio:4:1 loads rosin and isopropanol and sodium hydroxide with thermometer and blender and reflux dress
In the four-hole boiling flask put, it is put into water-bath and is heated to 60 DEG C, insulated and stirred 20min, then pine is added into four-hole boiling flask
The epoxychloropropane of the quality such as perfume (or spice) and the triethylamine of rosin quality 70%, unreacted is distilled to recover at 75 DEG C after back flow reaction 18h
Epoxychloropropane and triethylamine, obtain self fixing cationic rosin magma, weigh granatum and be put into tissue pulverizer and crush
20min, obtains granatum crushed material, is 1 in mass ratio by granatum crushed material and water:Mixed liquor is obtained after 20 mixing, then to
The sodium sulfite of granatum quality 0.5% is added in mixed liquor, oil bath heating is warming up to 100 DEG C of insulation extraction 3h, is separated by filtration
To filtrate, it is granatum extracting solution, is 1 in mass ratio by the sodium chloride solution that soybean and milk and mass fraction are 50%:
1:50 DEG C are heated to after 3 mixing, insulated and stirred extraction 40min, is separated by filtration removal filter residue, obtains protein extract, press
Parts by weight meter, weighs 30 portions of self fixing cationic rosin magmas, 10 parts of granatum extracting solutions, 8 parts of protein extracts and is sequentially loaded into band
Have in the three-necked flask of blender, startup blender is stirred 20min with 200r/min rotating speeds and obtains prefabricated solution, to above-mentioned dress
There are the trimethylborate that prefabricated solution quality 20% is added in the three-necked flask of prefabricated solution and the detergent alkylate sulphur of prefabricated solution quality 3%
Sour sodium, three-necked flask is moved into water-bath, is heated to 50 DEG C, is discharged after stirring reaction 1h, up to anti-current dehydration sill
Material preservative.
Example 2
It is 3 in mass ratio:4:1 loads rosin and isopropanol and sodium hydroxide with thermometer and blender and reflux dress
In the four-hole boiling flask put, it is put into water-bath and is heated to 65 DEG C, insulated and stirred 25min, then pine is added into four-hole boiling flask
The epoxychloropropane of the quality such as perfume (or spice) and the triethylamine of rosin quality 75%, unreacted is distilled to recover at 80 DEG C after back flow reaction 19h
Epoxychloropropane and triethylamine, obtain self fixing cationic rosin magma, weigh granatum and be put into tissue pulverizer and crush
25min, obtains granatum crushed material, is 1 in mass ratio by granatum crushed material and water:Mixed liquor is obtained after 20 mixing, then to
The sodium sulfite of granatum quality 0.6% is added in mixed liquor, oil bath heating is warming up to 103 DEG C of insulation extraction 4h, is separated by filtration
To filtrate, it is granatum extracting solution, is 1 in mass ratio by the sodium chloride solution that soybean and milk and mass fraction are 50%:
1:55 DEG C are heated to after 3 mixing, insulated and stirred extraction 50min, is separated by filtration removal filter residue, obtains protein extract, press
Parts by weight meter, weighs 35 portions of self fixing cationic rosin magmas, 13 parts of granatum extracting solutions, 9 parts of protein extracts and is sequentially loaded into band
Have in the three-necked flask of blender, startup blender is stirred 25min with 250r/min rotating speeds and obtains prefabricated solution, to above-mentioned dress
There are the trimethylborate that prefabricated solution quality 25% is added in the three-necked flask of prefabricated solution and the detergent alkylate sulphur of prefabricated solution quality 4%
Sour sodium, three-necked flask is moved into water-bath, is heated to 55 DEG C, is discharged after stirring reaction 1.5h, up to anti-current dehydration base
Timber preservative.
Example 3
It is 3 in mass ratio:4:1 loads rosin and isopropanol and sodium hydroxide with thermometer and blender and reflux dress
In the four-hole boiling flask put, it is put into water-bath and is heated to 70 DEG C, insulated and stirred 30min, then pine is added into four-hole boiling flask
The epoxychloropropane of the quality such as perfume (or spice) and the triethylamine of rosin quality 80%, unreacted is distilled to recover at 85 DEG C after back flow reaction 20h
Epoxychloropropane and triethylamine, obtain self fixing cationic rosin magma, weigh granatum and be put into tissue pulverizer and crush
30min, obtains granatum crushed material, is 1 in mass ratio by granatum crushed material and water:Mixed liquor is obtained after 20 mixing, then to
The sodium sulfite of granatum quality 0.8% is added in mixed liquor, oil bath heating is warming up to 105 DEG C of insulation extraction 5h, is separated by filtration
To filtrate, it is granatum extracting solution, is 1 in mass ratio by the sodium chloride solution that soybean and milk and mass fraction are 50%:
1:60 DEG C are heated to after 3 mixing, insulated and stirred extraction 60min, is separated by filtration removal filter residue, obtains protein extract, press
Parts by weight meter, weighs 40 portions of self fixing cationic rosin magmas, 15 parts of granatum extracting solutions, 10 parts of protein extracts and is sequentially loaded into band
Have in the three-necked flask of blender, startup blender is stirred 30min with 300r/min rotating speeds and obtains prefabricated solution, to above-mentioned dress
There are the trimethylborate that prefabricated solution quality 30% is added in the three-necked flask of prefabricated solution and the detergent alkylate sulphur of prefabricated solution quality 5%
Sour sodium, three-necked flask is moved into water-bath, is heated to 60 DEG C, is discharged after stirring reaction 2h, up to anti-current dehydration sill
Material preservative.
The timber preservative that comparative example is produced with company of Harbin City is as a comparison case to anti-current produced by the present invention
The timber preservative lost in aqueous wood preservative and comparative example is detected, and testing result is as shown in table 1：1st, test method
Method of the test method with reference to AWPAE11-2006.
Timber is absorbed after medicament dries 21 days, carries out indoor water leaching test, by sample packet distilled water immersion 14 days,
Refresh the water periodically and collect leachate, the fixation rate of medicament is calculated according to AWPAE11-97 standards.
Table 1
According to data in table 1, the fixation rate that borate in aqueous wood preservative is lost in anti-current produced by the present invention is high, has
The advantages of good penetrability, resistance leachability is strong, have wide prospect of the application.
Claims (6)
1. the preparation method of aqueous wood preservative is lost in a kind of anti-current, it is characterised in that specifically preparation process is：
（1）Rosin and isopropanol and sodium hydroxide are loaded and carry thermometer and the four-hole boiling flask of blender and reflux
In, heat temperature raising in water-bath, insulated and stirred are put into, then epoxychloropropane and triethylamine are added into four-hole boiling flask, reflux is anti-
Should after be distilled to recover unreacted epoxychloropropane and triethylamine, obtain self fixing cationic rosin magma；
（2）Weigh granatum and crush 20~30min, obtain granatum crushed material, obtained after granatum crushed material and water are mixed
Mixed liquor, then sodium sulfite is added into mixed liquor, oil bath heating heating, insulation 3~5h of extraction, is separated by filtration to obtain filtrate,
As granatum extracting solution；
（3）Heat temperature raising after soybean and milk and sodium chloride solution are mixed, insulated and stirred extract 40~60min, filtering point
Leave away and remove filter residue, obtain protein extract；
（4）Count in parts by weight, weigh 30~40 portions of self fixing cationic rosin magmas, 10~15 parts of granatum extracting solutions, 8~10 parts
Protein extract is sequentially loaded into the three-necked flask with blender, is started blender and is stirred to obtain prefabricated solution；
（5）Trimethylborate and neopelex are added into the above-mentioned three-necked flask equipped with prefabricated solution, by three mouthfuls of burnings
Bottle is moved into water-bath, heat temperature raising, discharges after 1~2h of stirring reaction, aqueous wood preservative is lost up to anti-current.
2. the preparation method of aqueous wood preservative is lost in a kind of anti-current according to claim 1, it is characterised in that：Step
（1）Described in rosin and the mass ratio of isopropanol and sodium hydroxide be 3:4:1, the temperature of heat temperature raising is 60~70 DEG C,
The insulated and stirred time is 20~30min, and the addition of epoxychloropropane is equal with rosin quality, and the addition of triethylamine is rosin
The 70~80% of quality, the temperature of back flow reaction is 75~85 DEG C, and the time of back flow reaction is 18~20h.
3. the preparation method of aqueous wood preservative is lost in a kind of anti-current according to claim 1, it is characterised in that：Step
（2）Described in granatum crushed material and water mass ratio be 1:20, the addition of sodium sulfite for granatum quality 0.5~
0.8%, the temperature of heat temperature raising is 100~105 DEG C.
4. the preparation method of aqueous wood preservative is lost in a kind of anti-current according to claim 1, it is characterised in that：Step
（3）Described in soybean and the mass ratio of milk and sodium chloride solution be 1:1:3, the mass fraction of sodium chloride solution is 50%,
The temperature of heat temperature raising is 50~60 DEG C.
5. the preparation method of aqueous wood preservative is lost in a kind of anti-current according to claim 1, it is characterised in that：Step
（4）Described in the rotating speed being stirred be 200~300r/min, the time being stirred is 20~30min.
6. the preparation method of aqueous wood preservative is lost in a kind of anti-current according to claim 1, it is characterised in that：Step
（5）Described in the addition of trimethylborate be the 20~30% of prefabricated solution quality, the addition of neopelex is
The 3~5% of prefabricated solution quality, the temperature of heat temperature raising is 50~60 DEG C, and the time for stirring reaction is 1~2h.
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Cited By (1)
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| CN108748530A (en) * | 2018-05-18 | 2018-11-06 | 俞小峰 | A kind of preparation method of mildew preventing agent for wood |
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