CN109206212A - A kind of preparation method of modified tung oil coated carbamide - Google Patents

A kind of preparation method of modified tung oil coated carbamide Download PDF

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Publication number
CN109206212A
CN109206212A CN201811072606.0A CN201811072606A CN109206212A CN 109206212 A CN109206212 A CN 109206212A CN 201811072606 A CN201811072606 A CN 201811072606A CN 109206212 A CN109206212 A CN 109206212A
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China
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tung oil
modified tung
modified
coated carbamide
preparation
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杜建军
黄帮裕
钟洛诚
王新爱
李永胜
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Zhongkai University of Agriculture and Engineering
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Zhongkai University of Agriculture and Engineering
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Priority to CN201811072606.0A priority Critical patent/CN109206212A/en
Publication of CN109206212A publication Critical patent/CN109206212A/en
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    • CCHEMISTRY; METALLURGY
    • C05FERTILISERS; MANUFACTURE THEREOF
    • C05CNITROGENOUS FERTILISERS
    • C05C9/00Fertilisers containing urea or urea compounds
    • CCHEMISTRY; METALLURGY
    • C05FERTILISERS; MANUFACTURE THEREOF
    • C05GMIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
    • C05G5/00Fertilisers characterised by their form
    • C05G5/30Layered or coated, e.g. dust-preventing coatings
    • CCHEMISTRY; METALLURGY
    • C05FERTILISERS; MANUFACTURE THEREOF
    • C05GMIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
    • C05G5/00Fertilisers characterised by their form
    • C05G5/30Layered or coated, e.g. dust-preventing coatings
    • C05G5/37Layered or coated, e.g. dust-preventing coatings layered or coated with a polymer

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Pest Control & Pesticides (AREA)
  • Paints Or Removers (AREA)

Abstract

The present invention provides a kind of preparation methods of modified tung oil coated carbamide, comprising: takes tung oil and modifying agent to mix, obtains modified tung oil;The modified tung oil is reacted with epoxychloropropane and catalyst heating, obtains modified tung oil carboxylate;It reacts the modified tung oil carboxylate to obtain modified tung oil ethylene oxidic ester with sodium hydroxide solution;The modified tung oil ethylene oxidic ester is mixed with curing agent and is made into coating liquid, and coating is carried out to urea by the coating liquid, obtains modified tung oil coated carbamide.The preparation method of modified tung oil coated carbamide provided by the present invention, simple process substantially increases biodegradability, extend slow-release time, and reduce production cost, for natural macromolecule modification epoxy resin integument slow-release fertilizer production, make and use and bring convenient and safety guarantee.

Description

A kind of preparation method of modified tung oil coated carbamide
Technical field
The invention belongs to technical field of polymer materials more particularly to a kind of preparation methods of modified tung oil coated carbamide.
Background technique
China has become maximum chemical fertilizer production and country of consumption in the world at present, however China's chemical fertilizer available nutrient utilizes Rate is not high, and chemical fertilizer wastage is big, and crop actual absorption amount is few, this not only brings huge wasting of resources economic loss, simultaneously Pollution of ecological environment.
In this context, slow release fertilizer becomes the sustainable development inevitable choice of agricultural.Slow release fertilizer refers to by one Fixed process means handle common fertilizer, delay the new-type fertilizer of nutrient releasing speed.Compared with common fertilizer, slow release fertilizer Nutrient element releasing rule more meet plant growth needs, existing research shows that slow release fertilizer not only saves manure resources, improves agriculture Industry production economy benefit, and can be reduced fertilizer application frequency, labour cost is reduced, while long-term fertilization can improve edaphon Environment increases land fertility.
Coated slow release fertilizer is one kind of slow release fertilizer, it is by wrapping one layer of obstacle hydrone on fertilizer core surface Material, slow down the speed that hydrone penetrates into core He dissolves nutrients, to delay the release of nutrient.According to coated fertilizer Type, coated slow release fertilizer be divided into natural polymer coating and synthesis macromolecule coating two major classes.
Existing natural macromolecule modification epoxy resin integument slow-release fertilizer preparation process is complicated, the processing cost of raw material is high It is high, and degradation effect is poor, slow-release time is short, is natural macromolecule modification epoxy resin to increase the burden of soil environment The production of film-coated and slow release fertilizer makes and uses and brings huge inconvenient and security risk.
Summary of the invention
In view of this, the present invention provides a kind of preparation method of modified tung oil coated carbamide to solve the prior art not Foot.
To solve the above problems, the present invention provides a kind of preparation method of modified tung oil coated carbamide, comprising:
It takes tung oil and modifying agent to mix, obtains modified tung oil;
The modified tung oil is reacted with epoxychloropropane and catalyst heating, obtains modified tung oil carboxylate;
It reacts the modified tung oil carboxylate to obtain modified tung oil ethylene oxidic ester with sodium hydroxide solution;
The modified tung oil ethylene oxidic ester is mixed with curing agent and is made into coating liquid, and by the coating liquid to urine Element carries out coating, obtains modified tung oil coated carbamide.
Preferably, described " taking tung oil and modifying agent to mix, to obtain modified tung oil " includes:
Taking parts by weight is that 10 parts of tung oil and 2-8 parts of modifying agent are mixed, and reacts 1-7 in 60-100 DEG C of heating Hour, the modified tung oil is obtained after vacuum distillation.
Preferably, the modifying agent is maleic anhydride, acrylic acid, polyacrylic acid, methyl acrylate, acrylic acid fourth One of ester, methyl methacrylate and unsaturated polyester (UP) are a variety of.
Preferably, described " modified tung oil to be reacted with epoxychloropropane and catalyst heating, obtains modified tung oil Carboxylate " includes:
By parts by weight be 10 parts the modified tung oil and 10-15 parts of epoxychloropropane and 0.1-0.5 parts urge Agent reacts 1-7 hours in 60-100 DEG C of heating, obtains modified tung oil carboxylate.
Preferably, the catalyst is cetyl trimethylammonium bromide, benzyltrimethylammonium chloride, benzyl triethyl ammonium One of ammonium chloride, tetrabutylammonium chloride and sodium bromide are a variety of.
Preferably, described " the modified tung oil carboxylate is reacted with sodium hydroxide solution obtain modified tung oil shrink it is sweet Grease " includes:
Take the modified tung oil ethylene oxidic ester and 0.2-1 parts of sodium hydroxide solution that parts by weight are 10 parts in 20- 60 DEG C of heating are reacted 1-7 hours, and the modified tung oil ethylene oxidic ester is obtained.
Preferably, the sodium hydroxide solution is the sodium hydroxide solution of 20-60wt%.
Preferably, the modified tung oil ethylene oxidic ester is the modified paulownia of epoxide number 0.413-0.481mol/100g Oily ethylene oxidic ester.
Preferably, described " the modified tung oil ethylene oxidic ester to be mixed with curing agent and is made into coating liquid, and passes through institute State coating liquid and coating carried out to urea, obtain modified tung oil coated carbamide " include:
Parts by weight are taken to be made into for 10 parts of the modified tung oil ethylene oxidic ester and the mixing of 2-6 parts of the curing agent Coating liquid;
At 60-100 DEG C, by the coating liquid to be rotated in the seed-coating machine after speed instillation preheating in 1-3mL/ minutes Urea surface, velocity of rotation is 10-25 revs/min in the seed-coating machine;
Every the dropwise addition of the 0.5-2 minutes pause coating liquids, continue to be added dropwise after the solidification of its coating, the coating liquid Quality is equivalent to the 4-6% of urea quality, obtains the modified tung oil coated carbamide.
Preferably, the curing agent is diethylenetriamine, triethylene tetramine, tetraethylenepentamine, maleic anhydride, neighbour One of phenyl dicarboxylic anhydride and phenyl tetrahydrophthalic anhydride are a variety of.
The present invention provides a kind of preparation method of modified tung oil coated carbamide, comprising: takes tung oil and modifying agent to mix, obtains To modified tung oil;The modified tung oil is reacted with epoxychloropropane and catalyst heating, obtains modified tung oil carboxylate;It will The modified tung oil carboxylate reacts to obtain modified tung oil ethylene oxidic ester with sodium hydroxide solution;The modified tung oil is contracted Water glyceride is mixed with curing agent is made into coating liquid, and carries out coating to urea by the coating liquid, obtains modified tung oil packet Film urea.Method provided by the invention, by carrying out the preparation of coated carbamide, modified tung oil with modified tung oil ethylene oxidic ester The epoxy terminated group of the high activity of ethylene oxidic ester and curing agent reaction time are short, and coating process is simple, while outer layer film hardness Height, wear-resisting property is good, is not easy to be damaged in transport and storage, reduces the proportion of goods damageds.With other epoxy resin integument fertilizer phases Than using tung oil to substantially increase biodegradable performance as natural polymer coated fertilizer in the present invention, more meeting green The requirement of agricultural, and reduce the cost of raw material.In short, the preparation method of modified tung oil coated carbamide provided by the present invention, Simple process substantially increases biodegradability, and reduces production cost, is natural macromolecule modification epoxy resin packet The production of film slow-release fertilizer makes and uses and brings convenient and safety guarantee.
Detailed description of the invention
Fig. 1 is the coated carbamide elution profiles signal of the preparation method embodiment 1 of modified tung oil coated carbamide of the present invention Figure;
Fig. 2 is the coated carbamide elution profiles signal of the preparation method embodiment 2 of modified tung oil coated carbamide of the present invention Figure;
Fig. 3 is the coated carbamide elution profiles signal of the preparation method embodiment 3 of modified tung oil coated carbamide of the present invention Figure;
Fig. 4 is the coated carbamide elution profiles signal of the preparation method embodiment 4 of modified tung oil coated carbamide of the present invention Figure;
Fig. 5 is the coated carbamide elution profiles signal of the preparation method embodiment 5 of modified tung oil coated carbamide of the present invention Figure.
The embodiments will be further described with reference to the accompanying drawings for the realization, the function and the advantages of the object of the present invention.
Specific embodiment
Mode combined with specific embodiments below is described in further detail technical solution of the present invention, but not Constitute any limitation of the invention, the modification of anyone limited times made within the scope of the invention as claimed, still at this Within the scope of the claims of invention.
The present invention provides a kind of preparation method of modified tung oil coated carbamide, comprising:
It takes tung oil and modifying agent to mix, obtains modified tung oil;
It is above-mentioned, it is to be understood that tung oil is a kind of excellent band dry vegetable oil, has fast drying, light specific gravity, light Damp degree is good, adhesive force is strong, heat-resisting, acidproof, alkaline-resisting, anti-corrosion, antirust, the characteristics such as non-conductive, degradable.It is manufacture paint, oil The primary raw material of ink is largely used as building, the waterproof of machinery, weapons, car and boat, fishing gear, electric appliance, anti-corrosion, antirusting paint, and can Make oilcloth, oilpaper, soap, pesticide etc..In the present invention, raw material is coated as the macromolecule of fertilizer.
The modified tung oil is reacted with epoxychloropropane and catalyst heating, obtains modified tung oil carboxylate;
It reacts the modified tung oil carboxylate to obtain modified tung oil ethylene oxidic ester with sodium hydroxide solution;
The modified tung oil ethylene oxidic ester is mixed with curing agent and is made into coating liquid, and by the coating liquid to urine Element carries out coating, obtains modified tung oil coated carbamide.
It is above-mentioned, after being modified tung oil, in a heated condition, modified tung oil and epoxychloropropane be catalyzed anti- It answers, then reaction product modified tung oil ethylene oxidic ester is reacted with sodium hydroxide solution, further reaction product is changed Property tung oil ethylene oxidic ester prepare coating liquid, and then by coating liquid to urea coated, to finally obtain modified tung oil coating Urea.
In addition, it is described " the modified tung oil carboxylate is reacted with sodium hydroxide solution obtain modified tung oil shrink it is sweet During grease ", sodium hydroxide solution could alternatively be sodium carbonate liquor, but preferably sodium hydroxide solution.It is carrying out instead During answering, to prevent sodium hydroxide solution from causing rouge hydrolysis, it can be reduced by carrying out ice bath to reaction raw materials Racemization of the sodium hydroxide as highly basic, improves the yield of reaction product.
In addition, tung oil-modified, or hydroxylating is hydrolyzed in tung oil under acidic environment, synthesizes paulownia oleyl alcohol Acid resin, and then the isocyanates of equivalent and tung oil based alkyd is taken to be reacted, obtain modified tung oil.
In addition, tung oil-modified, or 1,4 addition reactions occur using the conjugated double bond and bicyclopentadiene of tung oil, The unsaturated polyester resin of bicyclopentadiene sealing end, the resin and polystyrene are generated by free radical polymerization, obtains modified paulownia Oily (resin).
In addition, after tung oil and modifying agent are mixed, since the purity and tung oil of tung oil itself are made with reacting for modifying agent At impurity presence, such as acid anhydrides will affect further the catalysis of modified tung oil is reacted to a certain extent, make At the low yield of catalysis reaction, or a large amount of impurity are generated, to being had a certain impact for finished product.So " being taken described Tung oil and modifying agent mixing, obtain modified tung oil " the step of and it is described " by the modified tung oil and epoxychloropropane and catalysis Agent heating reaction, obtain modified tung oil carboxylate " the step of between, further modified tung oil can be purified, to remove Wherein a large amount of acid anhydrides carry out catalysis reaction to the modified tung oil for reaching certain purity, are greatly improved obtained by catalysis reaction Modified tung oil carboxylate yield, improve catalysis reaction efficiency, greatly reduce cost.Specific purification process, can be with To take the modified tung oil, being placed in organic solvent, extracted, obtain extract, then the extract is depressurized Distillation, obtains modified tung oil after purification.Wherein, extractant can be six alkane of Isosorbide-5-Nitrae-dioxy and water, and ratio can be 1:1 Or 2:1, extraction times can be 2-3 times, the temperature of vacuum distillation can be 60-70 DEG C.
Method provided by the invention, by carrying out the preparation of coated carbamide, modified tung oil with modified tung oil ethylene oxidic ester The epoxy terminated group of the high activity of ethylene oxidic ester and curing agent reaction time are short, and coating process is simple, while outer layer film hardness Height, wear-resisting property is good, is not easy to be damaged in transport and storage, reduces the proportion of goods damageds.With other epoxy resin integument fertilizer phases Than using tung oil to substantially increase biodegradable performance as natural polymer coated fertilizer in the present invention, more meeting green The requirement of agricultural, and reduce the cost of raw material.The present invention is modified to obtain modified tung oil by pure tung oil, to carry out To the coating of urea, which can realize direct biodegrade, with a large amount of nondegradable resinaes of addition in the prior art Compound is compared, and biodegradability is substantially increased.
In short, the preparation method of modified tung oil coated carbamide provided by the present invention, simple process substantially increase life Object degradation property extends slow-release time, reduces production cost as thin-film material using tung oil cheap, from a wealth of sources, For natural macromolecule modification epoxy resin integument slow-release fertilizer production, make and use and bring convenient and safety guarantee.
Preferably, described " taking tung oil and modifying agent to mix, to obtain modified tung oil " includes:
Taking parts by weight is that 10 parts of tung oil and 2-8 parts of modifying agent are mixed, and reacts 1-7 in 60-100 DEG C of heating Hour, the modified tung oil is obtained after vacuum distillation.
It is above-mentioned, the modifying agent be maleic anhydride, acrylic acid, polyacrylic acid, methyl acrylate, butyl acrylate, One of methyl methacrylate and unsaturated polyester (UP) are a variety of.
Preferably, the modifying agent is that maleic anhydride, acrylic acid, methyl acrylate are one or more.
Above-mentioned, modifying agent additive amount is the 20-80% of tung oil.
Above-mentioned, preparing modified tung oil is to the hybrid reaction of tung oil and modifying agent, specifically, modification procedure can be with are as follows: claim Parts by weight are taken to be stirred reaction 6 hours in 60 DEG C of connection for 25 parts of tung oil, 0.5 part of sodium hydroxide and 19 parts of methanol.Reaction It finishes, is slowly added dropwise after pH value is adjusted to 5~6 by a certain amount of glacial acetic acid, 50 parts of hexamethylene and 80 parts of water is first added, 30min is stood until being no longer layered after mixing, discards lower layer, and continues that the anhydrous sulphur of 1g is then added with 50mL water washing 2 times Sour sodium, overnight stand, filtering obtain tung oil methyl ester cyclohexane solution, and vacuum distillation removes hexamethylene at 85 DEG C, obtain bright orange Color liquid is tung oil methyl ester (TME).
Catalytic resin activation: resin first expands internal gutter sufficiently with 40 DEG C of 2~3h of distilled water immersion, then with 1% Wt chlorination sodium ethoxide solution immersion resin overnight and the cleaning of 50mL deionized water filter, then are placed in 10% sodium hydroxide solution and stir 5h and washing are mixed until filtrate is in neutrality, 10% sulfuric acid solution, which is added, in last past resin makes liquid level be higher by resin 5cm, stirs 2h And repetitive process ensures that ion exchange is complete three times, removes sulfuric acid solution and wash with distilled water until filtrate neutrality, is placed in yin Liang Chu sealing is spare.
Tung oil methyl ester is reacted with the D-A of maleic anhydride (MA): weigh 15 parts of TME, be added a certain amount of resin and MA is added solvent Isosorbide-5-Nitrae-six alkane of dioxy stirring until mixing completely, is passed through nitrogen 30min, it is certain to be heated to set temperature reaction Time, 110 DEG C of vacuum distillation 0.5h remove solvent and free acid value, are cooled to room temperature, and obtaining crocus liquid is Malaysia tung oil Acid anhydrides (MTA), as modified tung oil.
Preferably, described " modified tung oil to be reacted with epoxychloropropane and catalyst heating, obtains modified tung oil Carboxylate " includes:
By parts by weight be 10 parts the modified tung oil and 10-15 parts of epoxychloropropane and 0.1-0.5 parts Catalyst, 60-100 DEG C heating 1-7 hours, obtain modified tung oil carboxylate.
Preferably, the catalyst is cetyl trimethylammonium bromide, benzyltrimethylammonium chloride, benzyl triethyl ammonium One of ammonium chloride, tetrabutylammonium chloride and sodium bromide are a variety of.
It is above-mentioned, it is to be understood that epoxychloropropane is a kind of organic compound, is mainly applicable to asphalt mixtures modified by epoxy resin processed The stabilizer and chemical intermediate of rouge and a kind of oxygen carrier, the primary raw material of epoxy group and phenoxy resin;It manufactures sweet Oil;Cure propylene-based rubber;The solvent of cellulose esters and ether;The high wet-strength resins of paper industry.
Preferably, described " the modified tung oil carboxylate is reacted with sodium hydroxide solution obtain modified tung oil shrink it is sweet Grease " includes:
Take the modified tung oil ethylene oxidic ester and 0.2-1 parts of sodium hydroxide solution that parts by weight are 10 parts in 20- 60 DEG C of heating are reacted 1-7 hours, and the modified tung oil ethylene oxidic ester is obtained.
Preferably, the sodium hydroxide solution is the sodium hydroxide solution of 20-60wt%.
Above-mentioned, the sodium hydroxide solution can be sodium hydrate aqueous solution.Preferably, the modified tung oil shrinks sweet Grease is the modified tung oil ethylene oxidic ester of epoxide number 0.413-0.481mol/100g.
Preferably, described " the modified tung oil ethylene oxidic ester to be mixed with curing agent and is made into coating liquid, and passes through institute State coating liquid and coating carried out to urea, obtain modified tung oil coated carbamide " include:
Parts by weight are taken to be made into for 10 parts of the modified tung oil ethylene oxidic ester and the mixing of 2-6 parts of the curing agent Coating liquid;
At 60-100 DEG C, by the coating liquid to be rotated in the seed-coating machine after speed instillation preheating in 1-3mL/ minutes Urea surface, velocity of rotation is 10-25 revs/min in the seed-coating machine;
Every the dropwise addition of the 0.5-2.0 minutes pause coating liquids, continue to be added dropwise after the solidification of its coating, the coating Liquid quality is equivalent to the 4-6% of urea quality, obtains the modified tung oil coated carbamide.
Preferably, the curing agent is diethylenetriamine, triethylene tetramine, tetraethylenepentamine, maleic anhydride, neighbour One of phenyl dicarboxylic anhydride and phenyl tetrahydrophthalic anhydride are a variety of.
Above-mentioned, equipment used by coating of the present invention can be seed-coating machine.
Modified tung oil ethylene oxidic ester and curing agent stir evenly by a certain percentage is made into coating liquid, presses at 60~100 DEG C According to 1-3mL/ minutes plus coating liquid to the intracavitary preheating urea surface constantly rotated of seed-coating machine, rolling speed is 10-25 revs/min Clock is added coating liquid every stopping in 0.5-2 minutes, continuously adds coating liquid after its surface layer film sufficiently solidifies.Coating terminates, Obtain the smooth modified tung oil coated carbamide in surface.Coating liquid quality is the 4%-6% of urea quality, the nutrient of coated carbamide The sustained release phase was differed by 30 days to 80 days.
Above-mentioned, curing agent is diethylenetriamine, triethylene tetramine, tetraethylenepentamine, maleic anhydride, adjacent phenyl two Acid anhydrides, phenyl tetrahydrophthalic anhydride, dosage are the 20%-60% of modified tung oil ethylene oxidic ester.
To facilitate the understanding of the present invention, below with reference to embodiment to further illustrate the technical scheme of the present invention.Applicant Statement, detailed process equipment and process flow of the invention that the present invention is explained by the above embodiments, but the present invention not office It is limited to above-mentioned detailed process equipment and process flow, that is, does not mean that the present invention must rely on above-mentioned detailed process equipment and work Skill process could be implemented.It should be clear to those skilled in the art, any improvement in the present invention, produces to the present invention The equivalence replacement of each raw material of product and addition, the selection of concrete mode of auxiliary element etc., all fall within protection scope of the present invention and Within the open scope.
Data table related in the preparation method of modified tung oil coated carbamide in 1 embodiment 1-5 of table
Embodiment 1:
The present embodiment provides a kind of modified tung oil coated carbamides, the preparation method is as follows:
Step 1, it takes tung oil and modifying agent to be mixed according to preset ratio 1, is heated under the conditions of preset temperature 1 default Time 1 obtains the modified tung oil after vacuum distillation;
Step 2, the modified tung oil, epoxychloropropane and catalyst are mixed according to preset ratio 2, in preset temperature 2 Under the conditions of heat preset time 2, obtain modified tung oil carboxylate;
Step 3, take the modified tung oil ethylene oxidic ester and certain density sodium hydroxide solution according to preset ratio 3 It is mixed, heating reaction preset time 3, obtains the modified tung oil ethylene oxidic ester under the conditions of preset temperature 3;
Step 4, the modified tung oil ethylene oxidic ester and the curing agent is taken to be made into coating according to the mixing of preset ratio 4 Liquid;Under preset temperature 4, the coating liquid is centainly dripped to the urea surface for the rotation that speed is added after preheating, velocity of rotation is shown in Table 1;Every pause coating liquid interval time, suspend the dropwise addition of the coating liquid, continues to be added dropwise after the solidification of its coating, it is described Coating liquid quality is equivalent to urea quality and is shown in Table 1, obtains the modified tung oil coated carbamide.The coated carbamide nutrient slowly-released phase sees Table 1.
Embodiment 2:
The present invention provides a kind of modified tung oil coated carbamide, preparation method such as embodiment 1, specific raw material, adding proportion, The data such as parameter are shown in Table 1.
Embodiment 3:
The present invention provides a kind of modified tung oil coated carbamide, preparation method such as embodiment 1, specific raw material, adding proportion, The data such as parameter are shown in Table 1.
Embodiment 4:
The present invention provides a kind of modified tung oil coated carbamide, preparation method such as embodiment 1, specific raw material, adding proportion, The data such as parameter are shown in Table 1.
Embodiment 5:
The present invention provides a kind of modified tung oil coated carbamide, preparation method such as embodiment 1, specific raw material, adding proportion, The data such as parameter are shown in Table 1.
Experimental result:
By modified tung oil coated carbamide preparation method in embodiment 1-5, be prepared respectively with it is right in embodiment 1-5 The different modified tung oil coated carbamides answered.
With reference to Fig. 1, the coated carbamide of the embodiment 1-5 nutrient slowly-released phase is successively are as follows: 58 days, 70 days, 62 days, 54 days and 54 It, with it is existing using the urea product of tung oil coating compared with, reached more superior longer slow-release time.In short, The preparation method of modified tung oil coated carbamide provided by the present invention, simple process substantially increase biodegradability, prolong Long slow-release time, reduces production cost, is the production of natural macromolecule modification epoxy resin integument slow-release fertilizer, prepares and make With bringing convenient and safety guarantee.

Claims (10)

1. a kind of preparation method of modified tung oil coated carbamide, which is characterized in that including following component:
It takes tung oil and modifying agent to mix, obtains modified tung oil;
The modified tung oil is reacted with epoxychloropropane and catalyst heating, obtains modified tung oil carboxylate;
It reacts the modified tung oil carboxylate to obtain modified tung oil ethylene oxidic ester with sodium hydroxide solution;
The modified tung oil ethylene oxidic ester is mixed with curing agent and is made into coating liquid, and urea is carried out by the coating liquid Coating obtains modified tung oil coated carbamide.
2. the preparation method of modified tung oil coated carbamide as described in claim 1, which is characterized in that described " to take tung oil and modification Agent mixing, obtains modified tung oil " include:
Taking parts by weight is that 10 parts of tung oil and 2-8 part of modifying agent are mixed, 60-100 DEG C heating 1-7 hours, depressurize The modified tung oil is obtained after distillation.
3. the preparation method of modified tung oil coated carbamide as claimed in claim 2, which is characterized in that the modifying agent is maleic One in dicarboxylic anhydride, acrylic acid, polyacrylic acid, methyl acrylate, butyl acrylate, methyl methacrylate and unsaturated polyester (UP) Kind is a variety of.
4. the preparation method of modified tung oil coated carbamide as described in claim 1, which is characterized in that described " by the modified paulownia Oil is reacted with epoxychloropropane and catalyst heating, obtains modified tung oil carboxylate " include:
The modified tung oil and 10-15 parts of epoxychloropropane and 0.1-0.5 parts of catalysis by parts by weight for 10 parts Agent, 60-100 DEG C heating 1-7 hours, obtain modified tung oil carboxylate.
5. the preparation method of modified tung oil coated carbamide as described in any one of claim 1-4, which is characterized in that the catalysis Agent is cetyl trimethylammonium bromide, benzyltrimethylammonium chloride, benzyltriethylammoinium chloride, tetrabutylammonium chloride and bromination One of sodium is a variety of.
6. the preparation method of modified tung oil coated carbamide as described in claim 1, which is characterized in that described " by the modified paulownia Grease compound reacts to obtain modified tung oil ethylene oxidic ester with sodium hydroxide solution " include:
Take the modified tung oil carboxylate and 0.2-1 parts of sodium hydroxide solution that parts by weight are 10 parts in 20-60 DEG C of heating Reaction 1-7 hours, obtains the modified tung oil ethylene oxidic ester.
7. the preparation method of modified tung oil coated carbamide as claimed in claim 6, which is characterized in that the sodium hydroxide solution is The sodium hydroxide solution of 20-60wt%.
8. the preparation method of modified tung oil coated carbamide as described in claim 1, which is characterized in that the modified tung oil shrinks sweet Grease is the modified tung oil ethylene oxidic ester of epoxide number 0.413-0.481mol/100g.
9. the preparation method of modified tung oil coated carbamide as described in claim 1, which is characterized in that described " by the modified paulownia Oily ethylene oxidic ester is mixed with curing agent is made into coating liquid, and carries out coating to urea by the coating liquid, obtains modified paulownia Oily coated carbamide " includes:
Parts by weight are taken to be made into coating for 10 parts of the modified tung oil ethylene oxidic ester and the mixing of 2-6 parts of the curing agent Liquid;
Urea at 60-100 DEG C, by the coating liquid to be rotated in the seed-coating machine after speed instillation preheating in 1-3mL/ minutes Surface, velocity of rotation is 10-25 revs/min in the seed-coating machine;
Every the dropwise addition of the 0.5-2 minutes pause coating liquids, continue to be added dropwise after the solidification of its coating, the coating liquid quality phase When obtaining the modified tung oil coated carbamide in the 4-6% of urea quality.
10. the preparation method of modified tung oil coated carbamide as described in any one of 1,2,4 and 6-9 of claim, which is characterized in that The curing agent is diethylenetriamine, triethylene tetramine, tetraethylenepentamine, maleic anhydride, adjacent phenyl dicarboxylic anhydride and phenyl One of tetrahydrophthalic anhydride is a variety of.
CN201811072606.0A 2018-09-14 2018-09-14 A kind of preparation method of modified tung oil coated carbamide Pending CN109206212A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110343573A (en) * 2019-06-04 2019-10-18 仲恺农业工程学院 A kind of method of modifying of grease and its application

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