CN109809864A - A kind of preparation method of acylation chitosan slow-release fertilizer coating materials - Google Patents
A kind of preparation method of acylation chitosan slow-release fertilizer coating materials Download PDFInfo
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- CN109809864A CN109809864A CN201711150607.8A CN201711150607A CN109809864A CN 109809864 A CN109809864 A CN 109809864A CN 201711150607 A CN201711150607 A CN 201711150607A CN 109809864 A CN109809864 A CN 109809864A
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Abstract
The present invention provides a kind of preparation methods of acylation chitosan slow-release fertilizer coating materials in agricultural technology field, include the following steps, experimental raw is ready to spare by (1)；(2) preparation of acylation chitosan: will be in the 70mL mixed solution of 5g chitosan addition pyridine and chloroform 1:1(v/v); acyl chlorides is added dropwise in ice bath; control is added dropwise in 1h; reaction system is risen into certain temperature; after reaction, acylation chitosan crude product is obtained by filtration, acylation chitosan crude product is used into acetone extraction 8h in cable type extractor according; drying for 24 hours, obtains the acylation chitosan powder of different degree of substitution to acylation chitosan powder after extracting in a vacuum drying oven；(3) at the preparation of film liquid；(4) film forming procedure；The thermal stability of the coated fertilizer prepared with this preparation method is more preferable.
Description
Technical field
The present invention relates to chemical preparation techniques field, in particular to a kind of preparation of acylation chitosan slow-release fertilizer coating materials
Method.
Background technique
FAO (Food and Agriculture Organization of the United Nation) (AFO) statistics shows that in improving crop yield, chemical fertilizer role accounts for 40% 1
60%, with the growth of population and the reduction in arable land, Yao Zengjia grain yield meets needs of the population growth to grain, increaseization
Fertilizer investment is indispensable.But a large number of studies show that: this season utilization rate nitrogenous fertilizer of China's farmland fertilizer is only 3%-35%,
Phosphate fertilizer is 10%-20%, potash fertilizer 35%-50%, lower than external similar about 5-20 percentage points of fertilizer.By taking nitrogenous fertilizer as an example, every annual loss
The nitrogen quantity of mistake is equivalent to more than 1,900 ten thousand tons of urea, converts into more than 380 hundred million yuan of RMB.
From the aforegoing it can be seen that chemical fertilizer loss is a quite serious problem, direct economic loss is not only caused, but also
Greenhouse gas emission and water eutrophication are exacerbated, so the dirt for improving utilization rate of fertilizer, fertilizer being alleviated or avoided to environment
Dye, development continues, high-efficiency agriculture is the problem of people pay close attention to jointly, needs to produce novel fertilizer, to improve fertilizer utilization
Rate.
Summary of the invention
For the defects in the prior art, it is an object of the invention to solve the low technology of utilization rate of fertilizer in the prior art
Problem provides a kind of preparation method of acylation chitosan slow-release fertilizer coating materials, and utilization rate of fertilizer can be improved in the present invention, reduces ring
Border pollution.
The object of the present invention is achieved like this: a kind of preparation method of acylation chitosan slow-release fertilizer coating materials, including
Following steps,
(1) experimental raw is ready to spare；
(2) pyridine and chloroform 1:1(v/v the preparation of acylation chitosan: is added in 5g chitosan) 70mL mixed solution in, in ice
Acyl chlorides is added dropwise in bath, control is added dropwise in 1h, reaction system is risen to certain temperature, after reaction, acylation is obtained by filtration
Acylation chitosan crude product is used acetone extraction 8h, the acylation chitosan after extracting by chitosan crude product in cable type extractor according
Drying for 24 hours, obtains the acylation chitosan powder of different degree of substitution to powder in a vacuum drying oven；
(3) at the preparation of film liquid: measuring 50mL distilled water in beaker, add the glacial acetic acid of 1mL, be stirring evenly and then adding into 1g
Acylation chitosan powder continues stirring to acylation chitosan powder and is dissolved completely in aqueous acetic acid, at room temperature, stand for 24 hours with
Bubble is completely removed, for use；
(4) film forming procedure: different methods is selected to form a film according to different performance test.
As a further improvement of the present invention, the film in the step (4) for urea penetration testing is used with nylon cloth
Chitosan film is prepared for support, is specifically, one piece of smooth nylon grid cloth is placed on the smooth sheet glass of single side, it will be quiet
Chitosan solution after setting for 24 hours is added drop-wise to nylon filtering side, then with the coating device of same specification that chitosan solution is uniform
It is applied on nylon cloth, prepares the identical chitosan film of thickness, film is placed for 24 hours in 50 DEG C of vacuum ovens, solvent is complete
Volatilization obtains uniform, the identical chitosan film of thickness that forms a film, and chitosan film is put into dehydrated alcohol and impregnates 48h, washes away surface
Remaining acetic acid, then dry.
As a further improvement of the present invention, it is being cultivated in the step (4) for the film other than urea penetration testing
Curtain coating prepares chitosan film in ware, and specific step is to form a film in culture dish, and the solution of identical weight is poured into glass culture dish
In, it dried in 50 ' C vacuum ovens, take off film, the identical film of thickness is made.Film is impregnated into 48h in dehydrated alcohol, is washed away
Remained on surface acetic acid, then dry.
As a further improvement of the present invention, the experimental raw in the step (1) includes that the shell of MV=6.0*105/DD=97% is poly-
Sugar, 99% caprylyl chloride, 97% hard acyl chlorides, specification are analytically pure acetone, specification is analytically pure chloroform, specification is analysis
Pure glacial acetic acid.
Detailed description of the invention
Fig. 1 is the composition figure of experimental raw in the present invention.
Specific embodiment
A kind of preparation method of acylation chitosan slow-release fertilizer coating materials, includes the following steps,
(1) experimental raw is ready to spare；
(2) pyridine and chloroform 1:1(v/v the preparation of acylation chitosan: is added in 5g chitosan) 70mL mixed solution in, in ice
Acyl chlorides is added dropwise in bath, control is added dropwise in 1h, reaction system is risen to certain temperature, after reaction, acylation is obtained by filtration
Acylation chitosan crude product is used acetone extraction 8h, the acylation chitosan after extracting by chitosan crude product in cable type extractor according
Drying for 24 hours, obtains the acylation chitosan powder of different degree of substitution to powder in a vacuum drying oven；
(3) at the preparation of film liquid: measuring 50mL distilled water in beaker, add the glacial acetic acid of 1mL, be stirring evenly and then adding into 1g
Acylation chitosan powder continues stirring to acylation chitosan powder and is dissolved completely in aqueous acetic acid, at room temperature, stand for 24 hours with
Bubble is completely removed, for use；
(4) film forming procedure: the film for urea penetration testing, which is used, prepares chitosan film by support of nylon cloth, is specifically,
One piece of smooth nylon grid cloth is placed on the smooth sheet glass of single side, and the chitosan solution after standing for 24 hours is added drop-wise to Buddhist nun
Chitosan solution, is then uniformly applied on nylon cloth with the coating device of same specification, it is identical to prepare thickness by dragon filtering side
Chitosan film, film is placed for 24 hours in 50 DEG C of vacuum ovens, solvent volatilize completely obtain film forming uniformly, thickness it is identical
Chitosan film is put into dehydrated alcohol and impregnates 48h by chitosan film, washes away remained on surface acetic acid, then dry.
In the present embodiment, the experimental raw (as shown in Figure 1) in step (1) include MV=6.0*105/DD=97% chitosan,
99% caprylyl chloride, 97% hard acyl chlorides, specification are analytically pure acetone, specification is analytically pure chloroform, specification is that analysis is pure
Glacial acetic acid.
Compared with prior art, the present invention the technical effect having are as follows: (1) using pyridine and chloroform as mixed solvent, ice
Cruel chlorine is added dropwise under the conditions of bath, heating makes cruel chlorine and chitosan react, in caprylyl chloride and stearyl chloride and chitosan molecule
Amino, hydroxyl react, and have synthesized the acylation chitosan of different carbon chain lengths, successfully make and respectively go out acylation chitosan slow-release fertilizer packet
Membrane material；
(2) reaction condition can influence reacting for acyl chlorides and chitosan, and then influence to uglify the degree of substitution of chitosan；
(3) when degree of substitution increases, uglify solubility of the chitosan in spirit of vinegar and be gradually reduced, comprehensively consider acylation chitosan
Dissolubility and urea permeability select acylation chitosan of the degree of substitution within 0.07 as later period research material；
(4) compared with unmodified chitosan film, two kinds of acylation chitosan film water absorption rate declines increase, acylated shell with degree of substitution
The water absorption rate of glycan film gradually decreases, and the octanylated chitosan film water absorption rate that degree of substitution is 0.07 is minimum；
(5) increase with degree of substitution, the crystallinity decline of cruel acylation chitosan film, thermal stability reduces；
(6) when degree of substitution is identical, the thermal stability of stearoylation chitosan is lower than octanylated chitosan；
(7) compared with unmodified chitosan film, the urea infiltration capacity of two kinds of acylation chitosan films reduces；Increase with degree of substitution,
The urea of octanylated chitosan and stearoylation chitosan film accumulates infiltration capacity decline；When degree of substitution is to change 07, octanylated shell
Glycan film urea accumulation infiltration capacity is minimum, and osmotic effect is best, passes through the controllable chitosan of degree of substitution for digging acylation chitosan processed
The urea of film accumulates infiltration capacity；
(8) in summary performance test and characterization, octanylated chitosan film are more suitable for chitosan film slow-release fertilizer coating materials,
Degree of substitution is when changing 0.07, and it is minimum that urea accumulates infiltration capacity；Present invention can apply to prepare acylation chitosan slow-release fertilizer coating material
In the work of material.
Embodiment 2
A kind of preparation method of acylation chitosan slow-release fertilizer coating materials, includes the following steps,
(1) experimental raw is ready to spare；
(2) pyridine and chloroform 1:1(v/v the preparation of acylation chitosan: is added in 5g chitosan) 70mL mixed solution in, in ice
Acyl chlorides is added dropwise in bath, control is added dropwise in 1h, reaction system is risen to certain temperature, after reaction, acylation is obtained by filtration
Acylation chitosan crude product is used acetone extraction 8h, the acylation chitosan after extracting by chitosan crude product in cable type extractor according
Drying for 24 hours, obtains the acylation chitosan powder of different degree of substitution to powder in a vacuum drying oven；
(3) at the preparation of film liquid: measuring 50mL distilled water in beaker, add the glacial acetic acid of 1mL, be stirring evenly and then adding into 1g
Acylation chitosan powder continues stirring to acylation chitosan powder and is dissolved completely in aqueous acetic acid, at room temperature, stand for 24 hours with
Bubble is completely removed, for use；
(4) film forming procedure: for the film other than urea penetration testing, curtain coating prepares chitosan film in culture dish, specific to walk
Suddenly it is to form a film in culture dish, the solution of identical weight is poured into glass culture dish, dries, takes off in 50 ' C vacuum ovens
Film is made the identical film of thickness, film is impregnated 48h in dehydrated alcohol, washes away remained on surface acetic acid, then dry.
The present invention is not limited to the above embodiments, on the basis of technical solution disclosed by the invention, the skill of this field
For art personnel according to disclosed technology contents, one can be made to some of which technical characteristic by not needing creative labor
A little replacements and deformation, these replacements and deformation all fall in the scope of protection of the present invention.
Claims (4)
1. a kind of preparation method of acylation chitosan slow-release fertilizer coating materials, which is characterized in that include the following steps,
(1) experimental raw is ready to spare；
(2) pyridine and chloroform 1:1(v/v the preparation of acylation chitosan: is added in 5g chitosan) 70mL mixed solution in, in ice
Acyl chlorides is added dropwise in bath, control is added dropwise in 1h, reaction system is risen to certain temperature, after reaction, acylation is obtained by filtration
Acylation chitosan crude product is used acetone extraction 8h, the acylation chitosan after extracting by chitosan crude product in cable type extractor according
Drying for 24 hours, obtains the acylation chitosan powder of different degree of substitution to powder in a vacuum drying oven；
(3) at the preparation of film liquid: measuring 50mL distilled water in beaker, add the glacial acetic acid of 1mL, be stirring evenly and then adding into 1g
Acylation chitosan powder continues stirring to acylation chitosan powder and is dissolved completely in aqueous acetic acid, at room temperature, stand for 24 hours with
Bubble is completely removed, for use；
(4) film forming procedure: different methods is selected to form a film according to different performance test.
2. preparation method according to claim 1, which is characterized in that for urea penetration testing in the step (4)
Film, which is used, prepares chitosan film by support of nylon cloth, is specifically, placed on the smooth sheet glass of single side one piece it is smooth
Chitosan solution after standing for 24 hours is added drop-wise to nylon filtering side by nylon grid cloth, then will with the coating device of same specification
Chitosan solution is uniformly applied on nylon cloth, prepares the identical chitosan film of thickness, and film is put in 50 DEG C of vacuum ovens
It sets for 24 hours, solvent volatilizees completely obtains uniform, the identical chitosan film of thickness that forms a film, and chitosan film is put into dehydrated alcohol and is soaked
48h is steeped, washes away remained on surface acetic acid, then dry.
3. preparation method according to claim 2, which is characterized in that for being surveyed in addition to urea permeates in the step (4)
Film outside the examination curtain coating in culture dish prepares chitosan film, and specific step is to form a film in culture dish, by the solution of identical weight
It pours into glass culture dish, is dried in 50 ' C vacuum ovens, takes off film, the identical film of thickness is made；By film in dehydrated alcohol
Middle immersion 48h, washes away remained on surface acetic acid, then dry.
4. the preparation method of described in any item a kind of acylation chitosan slow-release fertilizer coating materials according to claim 1~3, special
Sign is, the experimental raw in the step (1) include the chitosan of MV=6.0*105/DD=97%, 99% caprylyl chloride, 97%
Hard acyl chlorides, specification are analytically pure acetone, specification is analytically pure chloroform, specification is analytically pure glacial acetic acid.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115124275A (en) * | 2022-06-27 | 2022-09-30 | 上海摩瑟尔科学技术有限公司 | Lithium silicate-based organic-inorganic composite concrete permeation protective agent |
-
2017
- 2017-11-18 CN CN201711150607.8A patent/CN109809864A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115124275A (en) * | 2022-06-27 | 2022-09-30 | 上海摩瑟尔科学技术有限公司 | Lithium silicate-based organic-inorganic composite concrete permeation protective agent |
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Application publication date: 20190528 |