CN107188672A - A kind of dimerization acid-based epoxy resins film-coated controlled release fertilizer and preparation method thereof - Google Patents
A kind of dimerization acid-based epoxy resins film-coated controlled release fertilizer and preparation method thereof Download PDFInfo
- Publication number
- CN107188672A CN107188672A CN201710393116.XA CN201710393116A CN107188672A CN 107188672 A CN107188672 A CN 107188672A CN 201710393116 A CN201710393116 A CN 201710393116A CN 107188672 A CN107188672 A CN 107188672A
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- China
- Prior art keywords
- epoxy resins
- release fertilizer
- based epoxy
- dimerization
- acid
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Classifications
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05C—NITROGENOUS FERTILISERS
- C05C9/00—Fertilisers containing urea or urea compounds
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES 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
- C05G5/00—Fertilisers characterised by their form
- C05G5/30—Layered or coated, e.g. dust-preventing coatings
- C05G5/38—Layered or coated, e.g. dust-preventing coatings layered or coated with wax or resins
Abstract
The present invention relates to a kind of dimerization acid-based epoxy resins film-coated controlled release fertilizer and preparation method thereof, first dimeric dibasic acid and epoxidation reagent are reacted dimerization acid derivative is made, then coating liquid is made after being well mixed dimerization acid derivative, modifying agent, anhydrides compound and catalyst by different proportion, then coating liquid is sprayed in fertiliser granulates surface in multiple times on a small quantity, solidify at 60 90 DEG C after about 5 minutes, you can dimerization acid-based epoxy resins film-coated controlled release fertilizer is made.The present invention is using dimeric dibasic acid as main membrane material, and its resource is renewable, and wide material sources are cheap, and membrane material can voluntarily degrade in soil, environmental protection.
Description
(1) technical field
The present invention relates to a kind of dimerization acid-based epoxy resins film-coated controlled release fertilizer and preparation method thereof, belong to release and release control fertilizer life
Production field.
(2) background technology
Chemical fertilizer is as the important means of production of agricultural development, and with being continuously increased for mankind's grain demand, chemical fertilizer is used
Amount is also growing.But at present, the utilization rate of nitrogen fertilizer of China is very low, the problems such as the wasting of resources and environmental pollution very
Seriously.Prove that film-coated controlled release fertilizer can increase substantially the utilization rate of fertilizer nutrient through research and lot of experiments base demonstration,
Be conducive to saving manure resources and preserve the ecological environment, improve the growth and development state of crop, improve the yield and quality of crop,
The environmental type development of Fertilizer Industry is realized to greatest extent.At present, the main component of most of coated fertilizers is oil
Chemical product, the high price of petrochemicals and constantly exhausted petroleum resources and after being manured into soil the problems such as difficult degradation, sternly
The sustainable development of coating controlled-release fertilizer is hindered again.Therefore, both at home and abroad in the urgent need to a kind of raw material is renewable, preparation technology is simple
The good film-coated controlled release fertilizer of single, degradable, controlled-release effect, to be widely applied in agricultural production.
Chinese patent document CN103342910A (application numbers：201310237033.3) disclose a kind of degradable photocuring
Coated fertilizer and its application in coating slowly/controlled releasing fertilizer；It includes by weight percentage：50~90% improved plant
Oily prepolymer, 5~45% reactive diluent and 1~5% light trigger.Prepared and wrapped using degradable photocuring coated fertilizer
The method of film slowly/controlled releasing fertilizer, comprises the following steps：By above-mentioned degradable photocuring coated fertilizer even application to granular fertilizer
Expect surface；Then solidify through ultraviolet light irradiation, obtain coating slowly/controlled releasing fertilizer.But, the coated fertilizer uses light trigger not
Only cost is high, and environment is unfriendly.Chinese patent document CN 103304772A (application numbers：201310261558.0) open
A kind of vegetable oil based polyurethane coating, release and release control fertilizer and preparation method thereof, the vegetable oil based polyurethane film-coated controlled release fertilizer
Preparation method comprises the following steps：1) granulated fertilizer is preheated；2) it is the vegetable oil containing 2-6 hydroxyl is more
First alcohol and isocyanates at least containing two isocyanatos form vegetable oil based polyurethane bag after heating and being well mixed
Film liquid；3) the vegetable oil based polyurethane coating liquid is sprayed in fertiliser granulates surface after preheat；Treat the plant oil base
Repeat to spray the vegetable oil based polyurethane coating liquid after the solidification of polyurethane coated liquid 2-10 times, obtain the poly- ammonia of plant oil base
Ester film-coated controlled release fertilizer.But, the controlled-release effect of the coated fertilizer is not good.
Dimeric dibasic acid is the polymer being polymerized by the unrighted acid of 18 carbon, and resource is renewable, wide material sources, valency
Lattice are cheap.There is more active group in dimeric dibasic acid structure, and strand is longer, so obtained dimerization acid-based epoxy resins
With good film-forming property, intensity is high, toughness is strong the characteristics of, and membrane material can voluntarily degrade in soil, environmental protection.Therefore,
It is primary raw material using dimeric dibasic acid, dimerization acid-based epoxy resins coating controlled-release fertilizer is prepared, with wide market prospects.
To sum up, current coated fertilizer water imbibition is stronger, causes its water resistance poor, and nutrients release effect is not good.Therefore,
The excellent coating controlled-release fertilizer of degradable, controlled-release effect is prepared using renewable resource, it is significant.
(3) content of the invention
In view of the shortcomings of the prior art, especially existing degradable coated fertilizer water resistance is poor, and intensity is more low to ask
Topic.A kind of raw material of present invention offer is renewable, nutrient controlled-release effect is excellent, cheap, preparation technology is simple, residual film easily drops
Solution, is suitable for dimerization acid-based epoxy resins coating controlled-release fertilizer and the preparation method quickly produced in enormous quantities.
Technical scheme is as follows：
A kind of dimerization acid-based epoxy resins coating controlled-release fertilizer, including coated fertilizer and fertiliser granulates, described coated fertilizer
Raw material composition including following mass parts：
1-3 parts of 40-60 parts of dimerization acid derivative, 30-50 parts of modifying agent, 9-15 parts of anhydrides compound and catalyst.
, according to the invention it is preferred to, the raw material reaction that described dimerization acid derivative includes following mass parts is made：
1-3 parts of 100-200 parts of dimeric dibasic acid, 100-200 parts of epoxidation reagent and catalyst；
It is preferred that, described epoxidation reagent is epoxychloropropane, expoxy propane or/and oxirane.
According to the present invention, described coated fertilizer prepares the catalyst used and dimerization acid derivative prepares the catalysis used
Agent is identical.It is preferred that, described catalyst is benzyltriethylammoinium chloride, dibutyl tin laurate, monomethyl imidazoles or two
Picoline.
, according to the invention it is preferred to, described dimerization acid derivative is prepared as follows obtaining：
After 100-200 parts of dimeric dibasic acids, 100-200 parts of epoxidation reagents and 1-3 parts of catalyst are well mixed, in 110-
After being reacted 1-3 hours at 130 DEG C, 50-70 DEG C is cooled to, sodium hydroxide is added and calcium oxide reacts 2-4 hours, suction filtration, filtrate
Dimerization acid derivative is produced after rotary evaporation；
It is preferred that, described sodium hydroxide or the addition of calcium oxide are the 10-20% of dimeric dibasic acid quality.
, according to the invention it is preferred to, described modifying agent is bisphenol A diglycidyl ether, epoxy resin E44 or/and ring
Oxygen tree fat E51.
, according to the invention it is preferred to, described anhydrides compound is maleic anhydride, HHPA or/and succinic anhydride.
, according to the invention it is preferred to, described fertiliser granulates particle diameter is 2-5mm；
It is preferred that, described fertiliser granulates are urea, ammonium sulfate, diammonium hydrogen phosphate, potassium chloride, ammonium nitrate, biphosphate
Ammonium, NPK composite fertilizers, nitrophosphate fertilizer, ammonium hydrogen carbonate, potassium sulfate or potassium nitrate.
, according to the invention it is preferred to, in described dimerization acid-based epoxy resins coating controlled-release fertilizer, coated fertilizer weight accounts for two
The 5.0-10.0% of polyacids base epoxy coating controlled-release fertilizer gross weight.
According to the present invention, the preparation method of described dimerization acid-based epoxy resins coating controlled-release fertilizer, including step are as follows：
Coating liquid is made after dimerization acid derivative, modifying agent, anhydrides compound and catalyst are well mixed, then will
Coating liquid sprays to fertiliser granulates surface, solidifies at 60-90 DEG C, produces dimerization acid-based epoxy resins coating controlled-release fertilizer.
According to the preparation method of Controlled Release Fertilizer of the present invention, it is preferred that coating liquid is sprayed several times, the amount sprayed every time will be lacked,
Spraying is uniform.
Beneficial effects of the present invention：
1. the coated fertilizer in the present invention is using dimeric dibasic acid as primary raw material, resource is renewable, and wide material sources, cost is low, and
And dimerization acid-based epoxy resins coated fertilizer has excellent water-resistance.
2. the present invention can be released by adjusting the formula of coated fertilizer and the coating rate of fertilizer, and then adjusting the nutrient of Controlled Release Fertilizer
The phase is put, the need for meeting different plant growths.
3. the coating controlled-release fertilizer that the present invention is prepared by primary raw material of dimeric dibasic acid, after nutrients release is complete, remains in soil
In putamina can voluntarily degrade, environmental protection.
(4) embodiment
With reference to specific embodiment, the present invention is further elaborated, but the present invention is not limited to following examples.Institute
It is conventional method unless otherwise instructed to state method.The material can be obtained from open commercial sources unless otherwise instructed.
Embodiment 1：
100g dimeric dibasic acids, 170g epoxychloropropane and 2g benzyltriethylammoinium chlorides are separately added into stirring in reactor makes
It is well mixed, after then being reacted 2 hours at 120 DEG C, is cooled to 60 DEG C, adds 10g sodium hydroxides and the reaction of 15g calcium oxide
3 hours, suction filtration produced dimerization acid derivative after rotary evaporation.Then by 4.33g dimerization acid derivative, 3.54g E44,0.87g
Sprayed to rapidly after maleic anhydride and 0.27g monomethyls imidazoles are well mixed and 60-90 DEG C of big of 500g is preheated in rotary drum
Grain urea granules surface.Film forming can be directly reacted in fertilizer surface after about 5 minutes, this process is repeated 3 times.Finally, fertilizer is passed through
Cooler is cooled to room temperature, you can packaging, storage.Gained Controlled Release Fertilizer membrane material accounts for 5% or so of whole Controlled Release Fertilizer gross weights.According to
《Slow release fertilizer》(GB/T 23348-2009) national standard and《Release and release control fertilizer》(HG/T 4215-2011) professional standard is surveyed
Examination, this fertilizer is in 25 DEG C of water or soil, and the nutrient control release time is about 85 days.
Embodiment 2：
140g dimeric dibasic acids, 170g epoxychloropropane and 3g dibutyl tin laurates are separately added into stirring in reactor makes
It is well mixed, after then being reacted 2 hours at 120 DEG C, is cooled to 60 DEG C, adds 15g sodium hydroxides and the reaction of 20g calcium oxide
3 hours, suction filtration produced dimerization acid derivative after rotary evaporation.Then by 4.63g dimerization acid derivative, 3.67g E44,0.85g
Sprayed to rapidly after maleic anhydride and 0.22g monomethyls imidazoles are well mixed and 60-90 DEG C of big of 500g is preheated in rotary drum
Grain urea granules surface.Film forming can be directly reacted in fertilizer surface after about 5 minutes, this process is repeated 3 times.Finally, fertilizer is passed through
Cooler is cooled to room temperature, you can packaging, storage.Gained Controlled Release Fertilizer membrane material accounts for 5% or so of whole Controlled Release Fertilizer gross weights.According to
《Slow release fertilizer》(GB/T 23348-2009) national standard and《Release and release control fertilizer》(HG/T 4215-2011) professional standard is surveyed
Examination, this fertilizer is in 25 DEG C of water or soil, and the nutrient control release time is about 65 days.
Embodiment 3：
120g dimeric dibasic acids, 150g expoxy propane and 1g benzyltriethylammoinium chlorides are separately added into stirring in reactor makes it
It is well mixed, after then being reacted 2 hours at 120 DEG C, 60 DEG C are cooled to, 15g sodium hydroxides and 15g calcium oxide reaction 3 is added
Dimerization acid derivative is produced after hour, suction filtration, rotary evaporation.Then 4.83g dimerization acid derivative, 3.55g bisphenol-As two are shunk
Sprayed to rapidly after glycerin ether, 0.88g HHPAs and 0.25g monomethyls imidazoles are well mixed and 60-90 is preheated in rotary drum
DEG C 500g granular urea particle surfaces.Film forming can be directly reacted in fertilizer surface after about 5 minutes, this process is repeated 3 times.
Finally, fertilizer is cooled to room temperature through cooler, you can packaging, storage.Gained Controlled Release Fertilizer membrane material accounts for whole Controlled Release Fertilizer gross weights
5% or so.According to《Slow release fertilizer》(GB/T 23348-2009) national standard and《Release and release control fertilizer》(HG/T 4215-2011) OK
Industry standard is tested, and this fertilizer is in 25 DEG C of water or soil, and the nutrient control release time is about 90 days.
Embodiment 4：
100g dimeric dibasic acids, 200g epoxychloropropane and 3g benzyltriethylammoinium chlorides are separately added into stirring in reactor makes
It is well mixed, after then being reacted 2 hours at 120 DEG C, is cooled to 60 DEG C, adds 15g sodium hydroxides and the reaction of 15g calcium oxide
3 hours, suction filtration produced dimerization acid derivative after rotary evaporation.Then 4.78g dimerization acid derivative, 3.44g bisphenol-As two are contracted
Sprayed to rapidly after water glycerin ether, 1.02g maleic anhydrides and 0.24g monomethyls imidazoles are well mixed and 60- is preheated in rotary drum
90 DEG C of 500g granular urea particle surfaces.Film forming can be directly reacted in fertilizer surface after about 5 minutes, this process repeats 4
It is secondary.Finally, fertilizer is cooled to room temperature through cooler, you can packaging, storage.Gained Controlled Release Fertilizer membrane material accounts for whole Controlled Release Fertilizer gross weights
7% or so.According to《Slow release fertilizer》(GB/T 23348-2009) national standard and《Release and release control fertilizer》(HG/T 4215-2011)
Professional standard is tested, and this fertilizer is in 25 DEG C of water or soil, and the nutrient control release time is about 152 days.
Embodiment 5：
150g dimeric dibasic acids, 150g epoxychloropropane and 3g benzyltriethylammoinium chlorides are separately added into stirring in reactor makes
It is well mixed, after then being reacted 2 hours at 120 DEG C, is cooled to 60 DEG C, adds 20g sodium hydroxides and the reaction of 20g calcium oxide
3 hours, suction filtration produced dimerization acid derivative after rotary evaporation.Then by 4.33g dimerization acid derivative, 3.27g E44,0.81g
Sprayed to rapidly after succinic anhydride and 0.20g lutidines are well mixed and 60-90 DEG C of big of 500g is preheated in rotary drum
Grain urea granules surface.Film forming can be directly reacted in fertilizer surface after about 5 minutes, this process is repeated 6 times.Finally, fertilizer is passed through
Cooler is cooled to room temperature, you can packaging, storage.Gained Controlled Release Fertilizer membrane material accounts for 9% or so of whole Controlled Release Fertilizer gross weights.According to
《Slow release fertilizer》(GB/T 23348-2009) national standard and《Release and release control fertilizer》(HG/T 4215-2011) professional standard is surveyed
Examination, this fertilizer is in 25 DEG C of water or soil, and the nutrient control release time is about 210 days.
Claims (10)
1. a kind of dimerization acid-based epoxy resins coating controlled-release fertilizer, including coated fertilizer and fertiliser granulates, it is characterised in that described
The raw material that coated fertilizer includes following mass parts is constituted：
1-3 parts of 40-60 parts of dimerization acid derivative, 30-50 parts of modifying agent, 9-15 parts of anhydrides compound and catalyst.
2. dimerization acid-based epoxy resins coating controlled-release fertilizer according to claim 1, it is characterised in that described dimeric dibasic acid spreads out
Raw material reaction of the biology including following mass parts is made：
1-3 parts of 100-200 parts of dimeric dibasic acid, 100-200 parts of epoxidation reagent and catalyst.
3. dimerization acid-based epoxy resins coating controlled-release fertilizer according to claim 2, it is characterised in that described epoxidation examination
Agent is epoxychloropropane, expoxy propane or/and oxirane.
4. dimerization acid-based epoxy resins coating controlled-release fertilizer according to claim 1 or 2, it is characterised in that described catalysis
Agent is benzyltriethylammoinium chloride, dibutyl tin laurate, monomethyl imidazoles or lutidines.
5. dimerization acid-based epoxy resins coating controlled-release fertilizer according to claim 1, it is characterised in that described dimeric dibasic acid spreads out
Biology is prepared as follows obtaining：
After 100-200 parts of dimeric dibasic acids, 100-200 parts of epoxidation reagents and 1-3 parts of catalyst are well mixed, at 110-130 DEG C
After lower reaction 1-3 hours, 50-70 DEG C is cooled to, sodium hydroxide is added and calcium oxide reacts 2-4 hours, suction filtration, filtrate rotation is steamed
Dimerization acid derivative is produced after hair.
6. dimerization acid-based epoxy resins coating controlled-release fertilizer according to claim 5, it is characterised in that described sodium hydroxide
Or the addition of calcium oxide is the 10-20% of dimeric dibasic acid quality.
7. dimerization acid-based epoxy resins coating controlled-release fertilizer according to claim 1, it is characterised in that described modifying agent is
Bisphenol A diglycidyl ether, epoxy resin E44 or/and epoxy resin E51；
It is preferred that, described anhydrides compound is maleic anhydride, HHPA or/and succinic anhydride.
8. dimerization acid-based epoxy resins coating controlled-release fertilizer according to claim 1, it is characterised in that described fertiliser granulates
Particle diameter is 2-5mm；
It is preferred that, described fertiliser granulates are urea, ammonium sulfate, diammonium hydrogen phosphate, potassium chloride, ammonium nitrate, ammonium dihydrogen phosphate,
NPK composite fertilizers, nitrophosphate fertilizer, ammonium hydrogen carbonate, potassium sulfate or potassium nitrate.
9. dimerization acid-based epoxy resins coating controlled-release fertilizer according to claim 1, it is characterised in that described dimerization acidic group
In epoxy resin integument Controlled Release Fertilizer, coated fertilizer weight accounts for the 5.0- of dimerization acid-based epoxy resins coating controlled-release fertilizer gross weight
10.0%.
10. the preparation method of the dimerization acid-based epoxy resins coating controlled-release fertilizer described in claim 1, including step are as follows：
Coating liquid is made after dimerization acid derivative, modifying agent, anhydrides compound and catalyst are well mixed, then by coating
Liquid sprays to fertiliser granulates surface, solidifies at 60-90 DEG C, produces dimerization acid-based epoxy resins coating controlled-release fertilizer.
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| CN201710393116.XA CN107188672A (en) | 2017-05-27 | 2017-05-27 | A kind of dimerization acid-based epoxy resins film-coated controlled release fertilizer and preparation method thereof |
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Application publication date: 20170922 |