CN107619641A - The method that microwave prepares tung oil coating - Google Patents
The method that microwave prepares tung oil coating Download PDFInfo
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- CN107619641A CN107619641A CN201710935094.5A CN201710935094A CN107619641A CN 107619641 A CN107619641 A CN 107619641A CN 201710935094 A CN201710935094 A CN 201710935094A CN 107619641 A CN107619641 A CN 107619641A
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- oil
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Abstract
The invention discloses a kind of method that microwave prepares tung oil coating, this method includes（1）Prepared by seed oil, the tung oil in paulownia seed is drawn using tung oil；（2）Prepared by washing oil, after the paulownia seed dregs of rice after seed oil and tung oil, water are mixed, continue hot-pressing, improve tung oil yield；（3）Tung oil coating preparation; washing oil and seed oil are mixed according to special ratios, after washed in saline solution, add epoxy resin and dihydric alcohol; heating response is carried out under microwave radiation technology; a kind of tung oil coating with high adhesion force is obtained, epoxy resin reacts with tung oil, after epoxy ring-opening; copolymer is formed with tung oil; increase adhesive force, dihydric alcohol can protect the acidic ingredients in tung oil, protect its bio-toxicity；The present invention obtains a kind of tung oil coating that is nuisanceless, not interfering with marine ecology, and this method preparation technology is simply controllable, suitable for industrial and scale.
Description
Technical field
The present invention relates to a kind of paint field, and in particular to a kind of method that microwave prepares tung oil coating.
Background technology
Several provinces in southwest abound with paulownia seed, and traditional method is that obtained tung oil is product, abandons oil cake（The paulownia seed dregs of rice）For waste.The paulownia seed dregs of rice
In fatty acidic materials, heavy dose of harmful, neural, digested system of bolt etc. in destruction, micro- dosage causes aquatic-organism
Brain god's bolt is firmly dead, is commonly called as plant " toxin ".
" tung oil coating " is also known as " flood oil ", refers to one kind and melts shape body coating, is to be fried to develop with paulownia seed dregs of rice pot with tung oil, former
Hunan Hongjiang is originated in, according to Historical Data Data About, between firstly appearing " Qing Dynasty's Jiaqing " year, existing more than 200 years history.It is mainly used in wooden article table
Face anti-corrosion, insect prevention, especially prevent that the adsorption effect of aquatic-organism is fine.Period most prevailing is on 1900-1935, Jiangsu and Zhejiang Provinces edge
Preferentially " flood oil " is used as anti-extra large clam coating to the band of sea one " the fish people ", though price is more expensive than tung oil a lot, effect is five times of tung oil.Boat
In salt water domain ship, just disembarkation removes extra large clam maintenance once to row typically more than 5 years." flood oil " not only domestic marketing, is also measured greatly
Mouth is external, is once praised by Foreign User（See nineteen twenty《U.S.'s commercial affairs report》）.As the development of history, wood ship are gradual
Disappear, " flood oil " because being eliminated steel body marine surface adhesive force is stranded, substitute it is the coating that ginseng has one kind " mercury chloride ".
But containing a large amount of metal ion mercury in mercury chloride coating, the pollution to seawater is very big, and a large amount of uses can destroy the ecology of ocean
System, influence the marine eco-environment.It is badly in need of a kind of nuisanceless, strong with the adhesive force of stainless steel material new coating at present.
The content of the invention
To solve the above problems, the present invention provides a kind of new tung oil coating, it is nuisanceless to seawater, and and stainless steel
The adhesive force of material is strong, while the tung oil coating of the present invention can also prevent extra large clam adsorbing boat bottom.
A kind of method that microwave prepares tung oil coating, is comprised the steps of：
1. prepared by seed oil：After paulownia seed is collected, impurity is abandoned in screening, drying moisture to 10%-20%, is crushed, and crosses 40 mesh sieves, is added suitable
In the 10%-30% of paulownia powder of seeds quality tung oil, heating, pot is fried, and temperature of charge is controlled at 140-160 DEG C, 40-60 points of stir-frying
Clock, squeezing, isolates tung oil and the paulownia seed dregs of rice；The paulownia seed dregs of rice are pulverized again, cross 40 mesh sieves, suitable quantity of water is added, moisture is reached 10%-
20%, heating kettle is fried, and temperature of charge is controlled at 140-160 DEG C, is stir-fried 40-60 minutes, squeezing, isolates tung oil and the paulownia seed dregs of rice.
Preferably, described seed oil preparation process, during stir-frying for the first time, when material is in brownish red, stir-frying is terminated；
During second stir-fries, terminate to stir-fry when material is in yellow black.
Preferably,, can be by several times if material has dust to kick up during stir-frying in described seed oil preparation process
Add a small amount of water wetting.
2. prepared by washing oil：The paulownia seed dregs of rice obtained by above-mentioned steps are pulverized, cross 40 mesh sieves, add tung oil, water mixing, stirring and
Even, heating kettle is fried, and temperature control stir-fries 40-60 minutes at 160-200 DEG C, squeezes while hot, isolate tung oil and the paulownia seed dregs of rice.
It is the 5%-15% equivalent to paulownia seed dregs of rice quality that preferable described washing oil process, which adds water,.The tung oil of addition is suitable
In the 30%-40% of paulownia seed dregs of rice quality.
3. tung oil coating preparation：Seed oil and washing oil are mixed, added equivalent to seed oil with the 30-50%'s of washing oil gross mass
Saline solution, 60-80 DEG C is heated to, stirs 30-60 minutes, be cooled to room temperature, standing separation, go abandon water layer；Oil reservoir is put into pot
Stirring, epoxy resin and dihydric alcohol are added, is heated to 200 DEG C under microwave radiation technology, constant temperature is tempered 1 to 2 hour under microwave radiation technology, cold
But to room temperature.
Preferably, described seed oil and washing oil mixed proportion are 1:2-4, brine concentration is 10- in described saline solution
40%。
Further, described epoxy resin addition is the 5-15% of oil reservoir gross mass；Described epoxy resin is bisphenol-A
Type epoxy resin.
Described dihydric alcohol is the dihydric alcohol that carbon atom is 8-12, and addition is the 2-4% of oil reservoir；
Further, described dihydric alcohol is 1,2- glycol n-decanes, 1,2- glycol -2- methylnonanes, 1,2- glycol dodecane
Base, 1,2- glycol undecyl, preferably 1,2- glycol n-decanes.
The method have the characteristics that providing a kind of method that microwave prepares tung oil coating, the present invention is by Oleum Verniciae fordii using specific
The brine It of concentration, easy Rongcheng part in salt solution is mainly removed, ensure that tung oil coating is insoluble in salt solution；Coating
The space mainly entered with rigid hull by coating molecule in rigid body surface, after desiccation, adhewsive action is played, the present invention adds
Epoxy resin, contain a large amount of epoxy radicals in epoxy resin, it is and easy into hydrogen bond collection unity in tung oil in acid condition after open loop
Conjunction forms a kind of firm copolymer, has very strong adhesive force.
Another feature of the present invention is addition dihydric alcohol, and it is acidic materials that tung oil, which expels the Main Ingredients and Appearance of extra large oyster, when long
Between easily occur combined reaction and activity decrease in the seawater of alkalescence, while it is fatty acid that the acidic materials in tung oil are most of
Composition, permanent be easily oxidized cause its denaturation, and the present invention adds dihydric alcohol and carries out condensation protection with eleostearic acid, in the basic conditions
Hydrolysis slowly disconnects, and discharges acidic materials；And the present invention uses dihydric alcohol of the carbon atom for 8-12, carbon atom is too small,
Binary alcohol-soluble and water-soluble is too strong, can form perforating agent, influences the effect of whole coating, and carbon atom is excessive, and hydrophobicity is too strong, not the Yishui River
Solution, acidic materials are difficult to discharge.
Compared with prior art, the beneficial effects of the present invention are：
1. it is nuisanceless to provide one kind, the natural plants coating of the aquatic-organisms such as extra large oyster can be removed.
2. the preparation method technique of the present invention is simply controllable, suitable for large-scale production and control.
The coating of gained of the invention has very strong adhesive force for rigid body ship, can replace current " chlorination completely
Mercury " coating.
Embodiment
The method for preparing tung oil coating to microwave below is described in detail.
Comparative example 1
1. prepared by seed oil：After paulownia seed is collected, decontamination is screened, drying moisture to 15%, is crushed, 40 mesh sieves is crossed, adds equivalent to paulownia
15% tung oil of powder of seeds quality, heating, pot are fried, and temperature of charge is controlled at 150 DEG C, are stir-fried 50 minutes, squeezing, isolate paulownia
Oil and the paulownia seed dregs of rice；The paulownia seed dregs of rice are pulverized again, cross 40 mesh sieves, add suitable quantity of water, moisture is reached 15%, heating kettle is fried, temperature of charge
Control stir-fries 50 minutes at 150 DEG C, squeezing, isolates tung oil and the paulownia seed dregs of rice.
2. prepared by washing oil：The paulownia seed dregs of rice obtained by above-mentioned steps are pulverized, cross 40 mesh sieves, add tung oil, water mixing, stirring and
Even, heating kettle is fried, and temperature control stir-fries 50 minutes at 180 DEG C, squeezes while hot, isolate tung oil and the paulownia seed dregs of rice.
3. tung oil coating preparation：Seed oil and washing oil are mixed, add 40% salt equivalent to seed oil and washing oil gross mass
Water, 70 DEG C are heated to, stir 45 minutes, be cooled to room temperature, standing separation, go abandon water layer；Oil reservoir is put into pot and stirred, and microwave is auxiliary
Help down and be heated to 200 DEG C, constant temperature is tempered 1.5 hours under microwave radiation technology, is cooled to room temperature.
Comparative example 2
1. prepared by seed oil：After paulownia seed is collected, decontamination is screened, drying moisture to 15%, is crushed, 40 mesh sieves is crossed, adds equivalent to paulownia
15% tung oil of powder of seeds quality, heating, pot are fried, and temperature of charge is controlled at 150 DEG C, are stir-fried 50 minutes, squeezing, isolate paulownia
Oil and the paulownia seed dregs of rice；The paulownia seed dregs of rice are pulverized again, cross 40 mesh sieves, add suitable quantity of water, moisture is reached 15%, heating kettle is fried, temperature of charge
Control stir-fries 50 minutes at 150 DEG C, squeezing, isolates tung oil and the paulownia seed dregs of rice.
2. prepared by washing oil：The paulownia seed dregs of rice obtained by above-mentioned steps are pulverized, cross 40 mesh sieves, add tung oil, water mixing, stirring and
Even, heating kettle is fried, and temperature control stir-fries 50 minutes at 180 DEG C, squeezes while hot, isolate tung oil and the paulownia seed dregs of rice.
3. tung oil coating preparation：Seed oil and washing oil are mixed, enters in pot and stirs, 200 DEG C are heated under microwave radiation technology, microwave
The lower constant temperature of auxiliary is tempered 1.5 hours, is cooled to room temperature.
Comparative example 3
1. prepared by seed oil：After paulownia seed is collected, decontamination is screened, drying moisture to 15%, is crushed, 40 mesh sieves is crossed, adds equivalent to paulownia
15% tung oil of powder of seeds quality, heating, pot are fried, and temperature of charge is controlled at 150 DEG C, are stir-fried 50 minutes, squeezing, isolate paulownia
Oil and the paulownia seed dregs of rice；The paulownia seed dregs of rice are pulverized again, cross 40 mesh sieves, add suitable quantity of water, moisture is reached 15%, heating kettle is fried, temperature of charge
Control stir-fries 50 minutes at 150 DEG C, squeezing, isolates tung oil and the paulownia seed dregs of rice.
2. prepared by washing oil：The paulownia seed dregs of rice obtained by above-mentioned steps are pulverized, cross 40 mesh sieves, add tung oil, water mixing, stirring and
Even, heating kettle is fried, and temperature control stir-fries 50 minutes at 180 DEG C, squeezes while hot, isolate tung oil and the paulownia seed dregs of rice.
3. tung oil coating preparation：Seed oil and washing oil are mixed, add 40% salt equivalent to seed oil and washing oil gross mass
Water, 70 DEG C are heated to, stir 45 minutes, be cooled to room temperature, standing separation, go abandon water layer；Oil reservoir is put into pot and stirred, and adds two
First alcohol, 200 DEG C is heated under microwave radiation technology, constant temperature is tempered 1.5 hours under microwave radiation technology, is cooled to room temperature.
Embodiment 1：
1. prepared by seed oil：After paulownia seed is collected, decontamination is screened, drying moisture to 15%, is crushed, 40 mesh sieves is crossed, adds equivalent to paulownia
15% tung oil of powder of seeds quality, heating, pot are fried, and temperature of charge is controlled at 150 DEG C, are stir-fried 50 minutes, squeezing, isolate paulownia
Oil and the paulownia seed dregs of rice；The paulownia seed dregs of rice are pulverized again, cross 40 mesh sieves, add suitable quantity of water, moisture is reached 15%, heating kettle is fried, temperature of charge
Control stir-fries 50 minutes at 150 DEG C, squeezing, isolates tung oil and the paulownia seed dregs of rice.
2. prepared by washing oil：The paulownia seed dregs of rice obtained by above-mentioned steps are pulverized, cross 40 mesh sieves, add tung oil, water mixing, stirring and
Even, heating kettle is fried, and temperature control stir-fries 50 minutes at 180 DEG C, squeezes while hot, isolate tung oil and the paulownia seed dregs of rice.
3. tung oil coating preparation：Seed oil and washing oil are mixed, add 40% salt equivalent to seed oil and washing oil gross mass
Water, 70 DEG C are heated to, stir 45 minutes, be cooled to room temperature, standing separation, go abandon water layer；Oil reservoir is put into pot and stirred, and adds ring
Oxygen tree fat and dihydric alcohol, 200 DEG C are heated under microwave radiation technology, constant temperature is tempered 1.5 hours under microwave radiation technology, is cooled to room temperature.
Embodiment 2
1. prepared by seed oil：After paulownia seed is collected, decontamination is screened, drying moisture to 10%, is crushed, 40 mesh sieves is crossed, adds equivalent to paulownia
10% tung oil of powder of seeds quality, heating, pot are fried, and temperature of charge is controlled at 140 DEG C, are stir-fried 40 minutes, squeezing, isolate paulownia
Oil and the paulownia seed dregs of rice；The paulownia seed dregs of rice are pulverized again, cross 40 mesh sieves, add suitable quantity of water, moisture is reached 10%, heating kettle is fried, temperature of charge
Control stir-fries 40 minutes at 140 DEG C, squeezing, isolates tung oil and the paulownia seed dregs of rice.
2. prepared by washing oil：The paulownia seed dregs of rice obtained by above-mentioned steps are pulverized, cross 40 mesh sieves, add tung oil, water mixing, stirring and
Even, heating kettle is fried, and temperature control stir-fries 40 minutes at 160 DEG C, squeezes while hot, isolate tung oil and the paulownia seed dregs of rice.
3. tung oil coating preparation：Seed oil and washing oil are mixed, add 30% salt equivalent to seed oil and washing oil gross mass
Water, 60 DEG C are heated to, stir 30 minutes, be cooled to room temperature, standing separation, go abandon water layer；Oil reservoir is put into pot and stirred, and adds ring
Oxygen tree fat and dihydric alcohol, 200 DEG C are heated under microwave radiation technology, constant temperature is tempered 1 hour under microwave radiation technology, is cooled to room temperature.
Embodiment 3
1. prepared by seed oil：After paulownia seed is collected, decontamination is screened, drying moisture to 20%, is crushed, 40 mesh sieves is crossed, adds equivalent to paulownia
30% tung oil of powder of seeds quality, heating, pot are fried, and temperature of charge is controlled at 160 DEG C, are stir-fried 60 minutes, squeezing, isolate paulownia
Oil and the paulownia seed dregs of rice；The paulownia seed dregs of rice are pulverized again, cross 40 mesh sieves, add suitable quantity of water, moisture is reached 20%, heating kettle is fried, temperature of charge
Control stir-fries 60 minutes at 160 DEG C, squeezing, isolates tung oil and the paulownia seed dregs of rice.
2. prepared by washing oil：The paulownia seed dregs of rice obtained by above-mentioned steps are pulverized, cross 40 mesh sieves, add tung oil, water mixing, stirring and
Even, heating kettle is fried, and temperature control stir-fries 60 minutes at 200 DEG C, squeezes while hot, isolate tung oil and the paulownia seed dregs of rice.
3. tung oil coating preparation：Seed oil and washing oil are mixed, add 50% salt equivalent to seed oil and washing oil gross mass
Water, 80 DEG C are heated to, stir 60 minutes, be cooled to room temperature, standing separation, go abandon water layer；Oil reservoir is put into pot and stirred, and adds ring
Oxygen tree fat and dihydric alcohol, 200 DEG C are heated under microwave radiation technology, constant temperature is tempered 2 hours under microwave radiation technology, is cooled to room temperature.
The adhesive force detection experiment of tung oil coating
According to standard《GB 1720-1979 paint film adhesion detection methods》In method, take comparative example 1 to 3 and embodiment
1 to 3 group each 5g of tung oil coating, is uniformly coated on model, according to《GB 1720-1979 paint film adhesion detection methods》, portray
Cycloid, detection mark position 1 to position 7, site location and standard《GB 1720-1979 paint film adhesion detection methods》In
Unanimously, the intact degree of film at each position is calculated, judges the adhesive force of comparative example 1-3 and embodiment 1-3 tung oil coating, as a result
It is as follows：
The intact degree of the paint film of 1 position 1 to position of table 7
| Embodiment | Comparative example 1 | Comparative example 2 | Comparative example 3 | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Position 1 | 23% | 21% | 13% | 90% | 93% | 92% |
| Position 2 | 38% | 37% | 30% | 95% | 92% | 96% |
| Position 3 | 50% | 52% | 55% | It is intact | It is intact | It is intact |
| Position 4 | 63% | 67% | 66% | It is intact | It is intact | It is intact |
| Position 5 | 78% | 79% | 75% | It is intact | It is intact | It is intact |
| Position 6 | 90% | 92% | 95% | It is intact | It is intact | It is intact |
| Position 7 | 93% | 97% | 96% | It is intact | It is intact | It is intact |
Analyze from the above, according to standard《GB 1720-1979 paint film adhesion detection methods》The intact degree in position 1 is judged to reach
It is primary standard to 70%, judges from result of the test, the gained tung oil of embodiment 1 to 3 paint adhesion is far above primary standard.
Above-described embodiment is not to make any formal limitation to the present invention, any those skilled in the art,
In the case of not departing from technical solution of the present invention scope, all technical solution of the present invention is done using the technology contents of the disclosure above
Go out many possible changes and modifications, or be revised as the equivalent embodiment of equivalent variations.Therefore, it is every without departing from the technology of the present invention
The content of scheme, according to the technology of the present invention essence to any simple modifications, equivalents, and modifications made for any of the above embodiments,
It should fall in the range of technical solution of the present invention protection.
Claims (7)
1. a kind of method that microwave prepares tung oil coating, is comprised the steps of：
（1）It is prepared by seed oil：After paulownia seed is collected, decontamination is screened, drying moisture to 10%-20%, is crushed, crosses 40 mesh sieves, adds phase
When the tung oil of the 10%-30% in paulownia powder of seeds quality, heating, pot is fried, and temperature of charge is controlled at 140-160 DEG C, 40-60 points of stir-frying
Clock, squeezing, isolates tung oil and the paulownia seed dregs of rice；The paulownia seed dregs of rice are pulverized again, cross 40 mesh sieves, suitable quantity of water is added, moisture is reached 10%-
20%, heating kettle is fried, and temperature of charge is controlled at 140-160 DEG C, is stir-fried 40-60 minutes, squeezing, isolates tung oil and the paulownia seed dregs of rice；
（2）It is prepared by washing oil：The paulownia seed dregs of rice obtained by above-mentioned steps are pulverized, cross 40 mesh sieves, tung oil, water mixing is added, stirs and even,
Heating kettle is fried, and temperature control stir-fries 40-60 minutes at 160-200 DEG C, squeezes while hot, isolate tung oil and the paulownia seed dregs of rice；
（3）Tung oil coating preparation：Seed oil and washing oil are mixed, add the salt of the 30-50% equivalent to seed oil and washing oil gross mass
Water, 60-80 DEG C is heated to, stirs 30-60 minutes, be cooled to room temperature, standing separation, go abandon water layer；Oil reservoir is put into pot and stirred,
Epoxy resin and dihydric alcohol are added, is heated to 200 DEG C under microwave radiation technology, constant temperature is tempered 1 to 2 hour under microwave radiation technology, is cooled to
Room temperature produces.
2. the method that microwave prepares tung oil coating according to claim 1, it is characterised in that described seed oil preparation process, the
During once stir-frying, when material is in brownish red, terminate stir-frying；During second stir-fries, tied when material is in yellow black
Beam stir-fries.
3. the method that microwave prepares tung oil coating according to claim 1, it is characterised in that during described washing oil, add
5%-15% of the water equivalent to paulownia seed dregs of rice quality.
4. the method that microwave prepares tung oil coating according to claim 1, it is characterised in that during described washing oil, add
Tung oil equivalent to paulownia seed dregs of rice quality 30%-40%.
5. the method that microwave prepares tung oil coating according to claim 1, it is characterised in that described tung oil coating preparation mistake
Cheng Zhong, seed oil and washing oil mixed proportion are 1:2-4.
6. the method that microwave prepares tung oil coating according to claim 1, it is characterised in that described epoxy resin addition
For the 5-15% of oil reservoir gross mass.
7. the method that microwave prepares tung oil coating according to claim 1, it is characterised in that described dihydric alcohol is carbon atom
For 8-12 dihydric alcohol.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102702915A (en) * | 2012-04-09 | 2012-10-03 | 益阳市华兴机械科技有限公司 | Metal surface protective agent and production method |
| CN105505563A (en) * | 2015-12-15 | 2016-04-20 | 湖南林邑新能源有限公司 | Acidic tung oil production technology |
| CN106590917A (en) * | 2016-12-23 | 2017-04-26 | 韦罡 | Preparing method and application of tung oil and applicationl |
-
2017
- 2017-10-10 CN CN201710935094.5A patent/CN107619641A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102702915A (en) * | 2012-04-09 | 2012-10-03 | 益阳市华兴机械科技有限公司 | Metal surface protective agent and production method |
| CN105505563A (en) * | 2015-12-15 | 2016-04-20 | 湖南林邑新能源有限公司 | Acidic tung oil production technology |
| CN106590917A (en) * | 2016-12-23 | 2017-04-26 | 韦罡 | Preparing method and application of tung oil and applicationl |
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