CN114097772A - Preparation method of amino-oligosaccharin aqueous solution - Google Patents
Preparation method of amino-oligosaccharin aqueous solution Download PDFInfo
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- CN114097772A CN114097772A CN202111326931.7A CN202111326931A CN114097772A CN 114097772 A CN114097772 A CN 114097772A CN 202111326931 A CN202111326931 A CN 202111326931A CN 114097772 A CN114097772 A CN 114097772A
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/02—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing liquids as carriers, diluents or solvents
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/02—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms
- A01N43/04—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom
- A01N43/14—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom six-membered rings
- A01N43/16—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom six-membered rings with oxygen as the ring hetero atom
Abstract
The invention relates to a preparation method of amino-oligosaccharin aqueous solution, which comprises the following steps: (1) adding 5-30 parts by weight of acid-soluble chitosan into 1000 parts by weight of 700-1000 parts by weight of lignite extracting solution, and stirring and dissolving to obtain a mixed solution; (2) heating the mixed solution to 48-52 ℃, and adding 100-350 parts by weight of H2O2Stirring for reaction to obtain degradation liquid; (3) and (4) rotationally separating the degradation liquid for 4-6 minutes, and taking supernatant to obtain 2-5% of amino-oligosaccharin aqueous solution in parts by mass. The beneficial effects are as follows: the degradation time is short, the amino-oligosaccharin is stable, the glucosamine is low in parts by mass, the preparation process is simple, the industrial chain of lignite quality classification utilization is extended, no emission is caused, and the method is suitable for industrial production and use.
Description
Technical Field
The invention relates to preparation of amino-oligosaccharin, in particular to a preparation method of an amino-oligosaccharin aqueous solution.
Background
The amino-oligosaccharin is oligosaccharide with D-glucosamine linked by beta-1.4 glycosidic bond, and is prepared by degrading chitin to obtain chitosan and then degrading, or is prepared by extracting low-toxicity bactericide by microbial fermentation. The amino-oligosaccharin can inhibit the growth of some pathogenic bacteria, influence the germination of fungal spores, induce the variation of hypha morphology, change of intraspore biochemistry and the like. Can excite the gene in the plant body, produce chitinase, glucanase, phytoalexin, PR protein and the like with disease-resistant function, has the function of activating cells, is beneficial to the recovery of the damaged plant, promotes the root and the seedling, enhances the stress resistance of crops, and promotes the growth and the development of the plants. The amino-oligosaccharin solution has the functions of killing virus, bacteria and fungi. It has strong preventing and killing effects on fungi, bacteria and viruses, and also has nourishing, regulating, detoxicating and antibacterial effects. Can be widely used for preventing and treating mosaic disease, lobular disease, spot disease, anthracnose, downy mildew, epidemic disease, gummy stem blight, yellow dwarf disease, rice blast, bacterial wilt, soft rot and other diseases caused by viruses, bacteria and fungi of fruit trees, vegetables, underground rhizomes, tobacco, traditional Chinese medicinal materials and grain and cotton crops.
The lignite extracting solution is a byproduct of the production process of high-moisture lignite by adopting a quality-grading comprehensive utilization technology, and the development and the application are still in a starting stage. At present, the production method of amino-oligosaccharin researched at home and abroad mainly adopts a chemical method, a physical method, an enzymatic method and a composite degradation method derived from three degradation methods. Amino-oligosaccharins are usually made by backbone cleavage using chitosan. With the development requirement of green agriculture, the demand of amino-oligosaccharin is increasing, and the traditional process for preparing amino-oligosaccharin by hydrolyzing chitosan consumes a large amount of auxiliary materials, and the generated emissions cause certain pollution to the environment and the yield is relatively low.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, and provides a preparation method of an amino-oligosaccharin aqueous solution, which has the advantages of short degradation time, complete degradation, simple process and no secondary discharge, based on a lignite extracting solution in a lignite drying and upgrading process.
The technical scheme of the preparation method of the amino-oligosaccharin aqueous solution provided by the invention is as follows:
a preparation method of amino-oligosaccharin aqueous solution comprises the following steps:
(1) adding 5-30 parts by weight of acid-soluble chitosan into 1000 parts by weight of 700-1000 parts by weight of lignite extracting solution, and stirring and dissolving to obtain a mixed solution;
(2) heating the mixed solution to 48-52 ℃, and adding 100-350 parts by weight of H2O2Stirring for reaction to obtain degradation liquid;
(3) and (4) rotationally separating the degradation liquid for 4-6 minutes, and taking supernatant to obtain 2-5% of amino-oligosaccharin aqueous solution in parts by mass.
Further, the total acid content of the lignite extracting solution is more than or equal to 0.6%, wherein the acetic acid content is more than or equal to 0.3%, the lignite extracting solution contains formic acid, acetic acid, propionic acid, butyric acid and isobutyric acid, and the pH value is 3.0-6.0.
Further, chitosan is CAS No.: 9012-76-4, and acid-soluble food-grade chitosan with deacetylation degree of 95%.
Further, H2O2The concentration is 3.6-4.6%.
Further, the reaction time in the step (2) is 3 to 5 hours.
Further, the rotational separation speed in the step (3) is 4000 rpm.
The implementation of the invention comprises the following technical effects:
the preparation method provided by the invention has the advantages of short degradation time, stable amino-oligosaccharin, low glucosamine mass fraction and simple preparation process, extends the industrial chain of lignite quality-based graded utilization, has no emission, and is suitable for industrial production and use. The lignite extracting solution is prepared by drying and upgrading lignite through high-temperature flue gas, and after lignite is graded according to quality, the lignite extracting solution is used as one of byproducts, so that the cost of raw materials is low.
Detailed Description
The present invention will be described in detail with reference to the following examples, which are intended to facilitate the understanding of the present invention and should not be construed as limiting in any way.
Example 1
The specific preparation method of the amino-oligosaccharin aqueous solution provided by the embodiment comprises the following steps:
(1) adding 5 parts by weight of acid-soluble chitosan into 700 parts by weight of lignite extracting solution, and stirring and dissolving to obtain a mixed solution;
(2) the mixture was heated to 50 ℃ and 115 parts by weight of H were added2O2Stirring the mixture to react for 4 hours, H2O2The concentration is 4% (W/V), and degradation liquid is obtained;
(3) and (3) rotationally separating the degradation liquid for 5 minutes at the rotational speed of 4000rpm, and taking supernate to obtain 2 +/-0.2 mass percent of amino-oligosaccharin aqueous solution.
Specifically, the lignite extracting solution is extracted by adopting a quality grading technology: the lignite raw material is crushed by the crusher and then conveyed to a vibrating screen through the scraper conveyor, and the vibrating screen screens out powdery lignite with set particle size; the method comprises the following steps of leading powdered lignite and high-temperature hot air with low oxygen content into a cavity of a drying device in a cocurrent mode, depolymerizing and dispersing the powdered lignite at a high speed in the drying device and enabling the powdered lignite to be in direct contact with the hot air to perform high-efficiency mass heat exchange, arranging an induced draft fan at the tail end of an air outlet of the drying device to enable the cavity of the drying device to generate negative pressure, leading out water smoke in the drying device under the action of the negative pressure, and condensing the water smoke to obtain lignite extracting solution after the water smoke is subjected to quality grading dust removal treatment. According to the above description, the skilled person can select the existing lignite drying and upgrading equipment according to the above steps, and the details are not repeated herein. In the embodiment, the total acid content of the lignite extracting solution is more than or equal to 0.6%, wherein the acetic acid content is more than or equal to 0.3%, the lignite extracting solution contains formic acid, acetic acid, propionic acid, butyric acid and isobutyric acid, and the pH value is 3.0-6.0. Chitosan in step (1), CAS No.: 9012-76-4, and acid-soluble food-grade chitosan with deacetylation degree of 95%. The preparation method of the amino-oligosaccharin aqueous solution provided by the invention has the advantages of short degradation time, stable amino-oligosaccharin, low glucosamine mass fraction and simple preparation process, extends the industrial chain of lignite quality-based graded utilization, has no emission, and is suitable for industrial production and use.
Example 2
The specific preparation method of the amino-oligosaccharin aqueous solution provided by the embodiment comprises the following steps:
(1) adding 15 parts by weight of acid-soluble chitosan into 800 parts by weight of lignite extracting solution, and stirring and dissolving to obtain a mixed solution;
(2) the mixture was heated to 45 ℃ and 215 parts by weight of H were added2O2Stirred for reaction for 3.5 hours, H2O2The concentration is 4.6% (W/V), and degradation liquid is obtained;
(3) and (4) rotationally separating the degradation liquid for 4 minutes at the rotational speed of 4000rpm, and taking supernatant to obtain 3 +/-0.2 mass percent of amino-oligosaccharin aqueous solution.
Example 3
The specific preparation method of the amino-oligosaccharin aqueous solution provided by the embodiment comprises the following steps:
(1) adding 20 parts by weight of acid-soluble chitosan into 900 parts by weight of lignite extracting solution, and stirring and dissolving to obtain a mixed solution;
(2) the mixture was heated to 55 ℃ and 260 parts by weight of H were added2O2Stirring the mixture to react for 5 hours, H2O2The concentration is 3.6% (W/V), and degradation liquid is obtained;
(3) and (4) carrying out rotary separation on the degradation liquid for 6 minutes at the rotation speed of 4000rpm, and taking supernate to obtain 4 +/-0.2% of amino-oligosaccharin aqueous solution in parts by mass.
Example 4
The specific preparation method of the amino-oligosaccharin aqueous solution provided by the embodiment comprises the following steps:
(1) adding 30 parts by weight of acid-soluble chitosan into 1000 parts by weight of lignite extracting solution, and stirring and dissolving to obtain a mixed solution;
(2) heating the mixed solution to 50 ℃, and adding 320 parts by weight of H2O2Stirring the mixture to react for 4 hours, H2O2The concentration is 4% (W/V), and degradation liquid is obtained;
(3) and (4) rotationally separating the degradation liquid for 4 minutes at the rotational speed of 4000rpm, and taking supernatant to obtain 5 +/-0.2% of amino-oligosaccharin aqueous solution.
The amino-oligosaccharin aqueous solutions prepared by the preparation methods of examples 1 to 4 were tested, and the test results are shown in the following table:
table 1 table of data of detection of amino-oligosaccharin aqueous solutions obtained in examples 1 to 4
| Numbering | Detecting items | Unit of | Example 1 | Example 2 | Example 3 | Example 4 | Basis of detection |
| 1 | Amino-oligosaccharin mass fraction | ％ | 1.9 | 3.1 | 3.9 | 5.1 | NY/T2889.2-2016 |
| 2 | Glucosamine mass fraction | ％ | 0.05 | 0.05 | 0.06 | 0.06 | NY/T2889.2-2016 |
| 3 | pH | / | 4.2 | 4.3 | 4.3 | 4.3 | NY/T2889.2-2016 |
| 4 | Water insoluble substance | ％ | 0.41 | 0.41 | 0.38 | 0.38 | NY/T2889.2-2016 |
The test data show that the preparation method of the amino-oligosaccharin aqueous solution has the advantages of stable amino-oligosaccharin mass fraction, high yield, lower glucosamine mass fraction and simple process steps.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the protection scope of the present invention, although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (6)
1. A preparation method of amino-oligosaccharin aqueous solution is characterized by comprising the following steps:
(1) adding 5-30 parts by weight of acid-soluble chitosan into 1000 parts by weight of 700-1000 parts by weight of lignite extracting solution, and stirring and dissolving to obtain a mixed solution;
(2) heating the mixed solution to 48-52 ℃, and adding 100-350 parts by weight of H2O2Stirring for reaction to obtain degradation liquid;
(3) and (4) rotationally separating the degradation liquid for 4-6 minutes, and taking supernatant to obtain 2-5% of amino-oligosaccharin aqueous solution in parts by mass.
2. The method of claim 1, wherein the lignite extract has a total acid content of 0.6% or more, an acetic acid content of 0.3% or more, a pH of 3.0-6.0, and contains formic acid, acetic acid, propionic acid, butyric acid and isobutyric acid.
3. The method for preparing an amino-oligosaccharin aqueous solution according to claim 1, wherein the chitosan is CAS no: 9012-76-4, and acid-soluble food-grade chitosan with deacetylation degree of 95%.
4. The method for producing an amino-oligosaccharin aqueous solution according to claim 1, wherein H is2O2The concentration is 3.6-4.6%.
5. The method for preparing an amino-oligosaccharin aqueous solution according to claim 1, wherein the reaction time in step (2) is 3 to 5 hours.
6. The method for preparing an amino-oligosaccharin aqueous solution according to claim 1, wherein the rotational separation speed in step (3) is 4000 rpm.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1654483A (en) * | 2005-01-26 | 2005-08-17 | 哈尔滨工业大学 | Process for preparing water-soluble chitosan oligosaccharide |
| CN102786607A (en) * | 2011-05-19 | 2012-11-21 | 浙江海洋学院 | Preparation method of water-soluble chitosan-oligosaccharide |
| US20200277408A1 (en) * | 2019-07-31 | 2020-09-03 | Jiangnan University | Anamylopectin-based Cyclic Glucan and Method for Processing the Same |
-
2021
- 2021-11-10 CN CN202111326931.7A patent/CN114097772A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1654483A (en) * | 2005-01-26 | 2005-08-17 | 哈尔滨工业大学 | Process for preparing water-soluble chitosan oligosaccharide |
| CN102786607A (en) * | 2011-05-19 | 2012-11-21 | 浙江海洋学院 | Preparation method of water-soluble chitosan-oligosaccharide |
| US20200277408A1 (en) * | 2019-07-31 | 2020-09-03 | Jiangnan University | Anamylopectin-based Cyclic Glucan and Method for Processing the Same |
Non-Patent Citations (1)
| Title |
|---|
| 王鹏云等: "褐煤提质分质分级利用技术及其产业化应用", 《中国煤炭》 * |
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