CN104725142A - Chitosan coating material with adjustable slow release performance and preparation method thereof - Google Patents
Chitosan coating material with adjustable slow release performance and preparation method thereof Download PDFInfo
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- CN104725142A CN104725142A CN201510132579.1A CN201510132579A CN104725142A CN 104725142 A CN104725142 A CN 104725142A CN 201510132579 A CN201510132579 A CN 201510132579A CN 104725142 A CN104725142 A CN 104725142A
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- Prior art keywords
- chitosan
- slow release
- blocked isocyanate
- mass ratio
- linking agent
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Classifications
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- 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
- C05G5/37—Layered or coated, e.g. dust-preventing coatings layered or coated with a polymer
Abstract
The invention discloses a chitosan coating material with adjustable slow release performance and a preparation method thereof. The method comprises the following steps: modifying the chitosan by the alkyl ketene dimers to obtain a hydrophobic chitosan slow release material, reacting the alkyl ketene dimers with active hydroxyl and amino in the chitosan chain and introducing a long-chain hydrophobic gene in the chitosan chain; and mixing a terminated isocyanate cross-linking agent and a modified chitosan derivative to prepare the slow release coating solution. The grafting ratio of the chitosan is different, the hydrophobic ability of the chitosan derivative is different, and the cross-linking degree of the material can be changed according to the dosage of the cross-linking agent, so that the slow release performance of the coating material can be adjusted and the purpose for adapting to different crop growth cycles can be reached.
Description
Technical field
The invention belongs to fertilizer slow release coating field, relate to chitosan coated material of a kind of adjustable sustained release performance and preparation method thereof.
Background technology
Nowadays the organic coated material category that fertilizer slow release coating is used is more, organic coated material has polymkeric substance (polyolefin resin, polyethylene, polystyrene, Synolac etc.), tar, rubber, latex, paraffin, pitch, oils etc., these organic materialss are difficult to regulate the sustained release performance of fertilizer can not degrade again, can pollute edatope.
Chitosan has very abundant biogenetic derivation, is biodegradable material.The fields such as medicine, tensio-active agent, parting material can be widely used in.Owing to chitosan chain there being the existence of a large amount of amino and hydroxyl, hydrophilic ability is comparatively by force, poor to the sustained release performance of fertilizer, chemically structure can change its hydrophilic and hydrophobic.The range of application of further expansion chitosan.
Summary of the invention
For the deficiencies in the prior art, the present invention proposes chitosan coated material of a kind of adjustable sustained release performance and preparation method thereof.
Chitosan relative molecular weight used in the present invention is 50 ~ 700,000, and deacetylation is 80 ~ 100%.
In the present invention, chitosan and alkyl ketene dimer react and carry out in suitable organic solvent, and solvent is the one in toluene, chloroform, ethylene dichloride, and the mass ratio of chitosan and solvent is 1:20.
In the present invention, chitosan is scattered in organic solvent, add alkyl ketene dimer and alkaline catalysts, chitosan and alkyl ketene dimer mass ratio are 4:1 ~ 1:5, alkaline catalysts is 1% ~ 3% of chitosan mass, be warming up to 70 ~ 120 DEG C, reaction 4 ~ 8h, be separated the dry chitosan derivatives obtaining hydrophobically modified.Blocked isocyanate linking agent and chitosan derivatives being dissolved in massfraction is be prepared into release-controlled coated liquid in the dilute acetic acid solution of 2 ~ 4%, the mass ratio of chitosan derivatives and blocked isocyanate is 20:1 ~ 10:1, blocked isocyanate linking agent is 2 ~ 3 functionality, deblocking temperature is 90 ~ 120 DEG C, and the mass ratio of chitosan derivatives and dilute acetic acid solution is 1:50 ~ 2:25.
In the present invention, chitosan and alkyl ketene dimer reaction, introduce chain hydrophobic side base.But chitosan does not still reach the requirement of fertilizer slow release coating, adds blocked isocyanate, add the isocyanic ester after thermal deblocking, make chitosan crosslinked, regulate the sustained release performance of material further, the requirement of fertilizer slow release coating can be reached.Release-controlled coated material preparation process in the present invention is simple.The mass ratio of chitosan and alkyl ketene dimer is regulated to regulate the percentage of grafting of chitosan, the mass ratio of chitosan derivatives and blocked isocyanate is regulated to regulate the crosslinking degree of material, sustained release performance regulates and controls by the percentage of grafting and crosslinking degree regulating chitosan, different crops growth needs can be met, and this type of release-controlled coated material belongs to degradation material, the pollution to edatope can be reduced, improve the utilization ratio of fertilizer.
Embodiment
below in conjunction with way of example, the present invention is described in further detail.
Embodiment one
The modification of step 1. chitosan: 6g chitosan is scattered in toluene solvant, and be stirred to evenly, add butyl ketene dimer 5g, 0.06g sodium hydroxide, reaction is warming up to 70 DEG C, reaction 4h.Reaction terminates to be separated drying and obtains chitosan derivatives.
2g chitosan derivatives and 0.17g blocked isocyanate are dissolved in the dilute acetic acid solution of 100g2% by step 2., obtain release-controlled coated liquid.
Embodiment two
6g chitosan is scattered in chloroform solvent by step 1., and is stirred to evenly, and add dodecylene ketone dimer 10g, 0.12g sodium hydroxide, is warming up to 90 DEG C, reaction 5h.Reaction terminates rear separation drying and obtains chitosan derivatives.
2g chitosan derivatives and 0.15g blocked isocyanate are dissolved in the dilute acetic acid solution of 100g2% by step 2., obtain release-controlled coated liquid.
Embodiment three
6g chitosan is scattered in toluene solvant by step 1., and is stirred to evenly, and add tetradecene ketone dimer 12g, 0.18g potassium hydroxide, is warming up to 100 DEG C, reaction 6h.Reaction terminates to be separated drying and obtains chitosan derivatives.
2g chitosan derivatives and 0.13g blocked isocyanate are dissolved in the dilute acetic acid solution of 100g2% by step 2., obtain release-controlled coated liquid.
Embodiment four
6g chitosan is scattered in toluene solvant by step 1., and is stirred to evenly, and add cetene ketone dimer 14g, 0.18g sodium hydroxide, is warming up to 110 DEG C, reaction 6h.Reaction terminates rear separation drying and obtains chitosan derivatives.
2g chitosan derivatives and 0.1g blocked isocyanate are dissolved in the dilute acetic acid solution of 100g2% by step 2., obtain release-controlled coated liquid.
Claims (9)
1. the chitosan coated material and preparation method thereof of an adjustable sustained release performance, that chitosan is scattered in organic solvent, add alkyl ketene dimer and alkaline catalysts, intensification reacting by heating for some time, be separated the dry chitosan derivatives obtaining hydrophobically modified, chitosan derivatives and the mixing of blocked isocyanate linking agent be dissolved in dilute acetic acid solution and be prepared into release-controlled coated liquid.
2., according to method according to claim 1, it is characterized in that the general structure of alkyl ketene dimer is:
Wherein, R, R
'it is the alkyl chain of 4 ~ 16 carbon.
3., according to method according to claim 1, it is characterized in that the molecular weight of chitosan is 50 ~ 700,000, deacetylation is 80 ~ 100%.
4., according to method according to claim 1, it is characterized in that reacting is carry out in toluene, chloroform, methylene dichloride a kind of organic solvent wherein, and the mass ratio of chitosan and solvent is 1:20.
5., according to method according to claim 1, it is characterized in that chitosan and alkyl ketene dimer mass ratio are 4:1 ~ 1:5.
6., according to method according to claim 1, it is characterized in that the temperature of reacting is 70 ~ 120 DEG C, the reaction times is 4 ~ 8h.
7., according to method according to claim 1, it is characterized in that the alkaline catalysts added is 1% ~ 3% of chitosan mass, wherein alkaline catalysts is the one in sodium hydroxide, potassium hydroxide.
8., according to method according to claim 1, it is characterized in that the blocked isocyanate linking agent used is 2 ~ 3 functionality, and deblocking temperature is 90 ~ 120 DEG C, the mass ratio of chitosan and blocked isocyanate is 20:1 ~ 10:1.
9., according to method according to claim 1, it is characterized in that chitosan derivatives and blocked isocyanate linking agent are dissolved in massfraction is in the dilute acetic acid solution of 2 ~ 4%, and the mass ratio of chitosan derivatives and dilute acetic acid is 1:50 ~ 2:25.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510132579.1A CN104725142B (en) | 2015-03-25 | 2015-03-25 | A kind of chitosan coated material of adjustable sustained release performance and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510132579.1A CN104725142B (en) | 2015-03-25 | 2015-03-25 | A kind of chitosan coated material of adjustable sustained release performance and preparation method thereof |
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| Publication Number | Publication Date |
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| CN104725142A true CN104725142A (en) | 2015-06-24 |
| CN104725142B CN104725142B (en) | 2017-12-19 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510132579.1A Expired - Fee Related CN104725142B (en) | 2015-03-25 | 2015-03-25 | A kind of chitosan coated material of adjustable sustained release performance and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107793228A (en) * | 2017-11-21 | 2018-03-13 | 常州创索新材料科技有限公司 | A kind of preparation method of the hydrophobic coated fertilizer of biodegradation type |
| CN111484373A (en) * | 2020-06-11 | 2020-08-04 | 福建师范大学 | Preparation method of slow-release fertilizer coating liquid using alkyl ketene dimer |
| CN114181015A (en) * | 2021-12-30 | 2022-03-15 | 中农金瑞肥业有限公司 | Composite slow-release compound fertilizer special for wheat and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1621455A (en) * | 2004-10-14 | 2005-06-01 | 武汉理工大学 | Method for preparing hydrophobic inorganic and organic composite corpuscle |
| CN101631838A (en) * | 2007-02-19 | 2010-01-20 | 西洛芬股份公司 | The polymeric film or the coating that comprise hemicellulose |
| CN101942780A (en) * | 2010-09-15 | 2011-01-12 | 山东轻工业学院 | Method for preparing AKD emulsion sizing agent |
-
2015
- 2015-03-25 CN CN201510132579.1A patent/CN104725142B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1621455A (en) * | 2004-10-14 | 2005-06-01 | 武汉理工大学 | Method for preparing hydrophobic inorganic and organic composite corpuscle |
| CN101631838A (en) * | 2007-02-19 | 2010-01-20 | 西洛芬股份公司 | The polymeric film or the coating that comprise hemicellulose |
| CN101942780A (en) * | 2010-09-15 | 2011-01-12 | 山东轻工业学院 | Method for preparing AKD emulsion sizing agent |
Non-Patent Citations (3)
| Title |
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| 杨媛等: "新型生物降解交联剂的制备和交联壳聚糖的性能", 《材料研究学报》 * |
| 薛贝等: "烷基烯酮二聚体改性瓜尔胶的制备及应用", 《中国造纸》 * |
| 陈强等: "可生物降解的壳聚糖肥料包膜材料的研究", 《高分子材料科学与工程》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107793228A (en) * | 2017-11-21 | 2018-03-13 | 常州创索新材料科技有限公司 | A kind of preparation method of the hydrophobic coated fertilizer of biodegradation type |
| CN111484373A (en) * | 2020-06-11 | 2020-08-04 | 福建师范大学 | Preparation method of slow-release fertilizer coating liquid using alkyl ketene dimer |
| CN114181015A (en) * | 2021-12-30 | 2022-03-15 | 中农金瑞肥业有限公司 | Composite slow-release compound fertilizer special for wheat and preparation method thereof |
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| CN104725142B (en) | 2017-12-19 |
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Granted publication date: 20171219 Termination date: 20210325 |