CN104782622A - Hydrogen sulfide slow-release inhibitor as well as preparation method and application thereof - Google Patents

Hydrogen sulfide slow-release inhibitor as well as preparation method and application thereof Download PDF

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CN104782622A
CN104782622A CN201510217662.9A CN201510217662A CN104782622A CN 104782622 A CN104782622 A CN 104782622A CN 201510217662 A CN201510217662 A CN 201510217662A CN 104782622 A CN104782622 A CN 104782622A
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paraffin
sustained release
release agent
nahs
preparation
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CN201510217662.9A
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CN104782622B (en
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金竹萍
裴雁曦
张丽萍
马晓丽
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Saixikang Shaanxi Biotechnology Co ltd
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Shanxi University
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Abstract

The invention discloses a hydrogen sulfide slow-release inhibitor as well as a preparation method and an application thereof. The method comprises the following steps: respectively dissolving a hydrogen sulfide donor such as sodium bisulfide (NaHS) and a coating agent into absolute ethyl alcohol, mixing and swirly mixing to obtain a mixed solution; adding the mixed solution into fused paraffin, ultrasonically mixing to obtain a paraffin solution containing the NaHS and the coating agent; dipping the paraffin solution into cold water to obtain a paraffin globule, cooling and drying to obtain the hydrogen sulfide slow-release inhibitor, wherein the mass ratio of the NaHS, the coating agent, the absolute ethyl alcohol to the paraffin is (0.5-5%): (1.5-15%): (5-20%): (60-93%). By adopting an ultrasonic-assisted dispersion technology, the mutual diffusion efficiency and effect of two solvents are improved. The concentration and the speed for releasing the H2S by the prepared slow-release inhibitor are stable and controllable and the slow-release inhibitor has an obvious promoting effect for the plant growth.

Description

A kind of hydrogen sulphide sustained release agent and its preparation method and application
Technical field:
The present invention relates to sustained release agent, specifically relate to a kind of hydrogen sulphide sustained release agent and its preparation method and application.
Background technology:
Hydrogen sulphide (H 2s) as the third gaseous signal molecule, there is comparatively deep research in animal body, proved the H of physiological concentration 2s almost participates in all vital movement processes: cardioprotection, vasodilator; suppress vascular smooth muscle cell proliferation, induction of vascular Vascular Smooth Muscle Cell Apoptosis, promote proliferation of microvascular endothelial cells, improve the multiple regulatory functions such as heart failure, diabetes, cirrhosis, septicemia, asthma.In recent years, H 2the research of S in plant corpus also achieves certain progress, finds that it can promote seed germination, root morphology builds up, and strengthen photosynthesis, adjustment is bloomed, and delays senility, increase yield etc.
At present about H 2the research of S physiological function in vivo, mainly carries out based on some pharmacology experiments.By with H 2the medicine donor process experiment material of S, observes and measures corresponding situation of change in material bodies.The most frequently used H 2s donor is NaHS (NaHS), can produce H after water-soluble 2s gas.The i.e. sulphur hydrogen radical ion (HS of NaHS -) with water in hydrogen ion (H +) combine and release H 2s, concrete reaction equation is: HS -+ H +=H 2s, and this course of reaction is very fast.
Based on H 2the characteristic that S low concentration is useful, high concentration is poisonous, is utilizing H 2during S gas treatment biomaterial often a micro-dosage continue process.Therefore, in actual mechanical process, be all generally the NaHS mother liquor preparing higher concentration in first closed container, and then dilute in proportion.Due to H 2the volatility of S, above operation not only cannot accurately control its concentration, and the repeatability of experiment reduces greatly; Also there is waste greatly, each actual NaHS used is only the some thousandths of of preparation mother liquor simultaneously.Therefore a kind of H of research and development is badly in need of 2s sustained release agent, meets the application demand of scientific experiment and agricultural production.
Summary of the invention:
The object of the invention is to overcome the H existed in prior art 2s concentration is wayward, the defect that availability is not high, provides a kind of stable performance, quality controllable H 2s sustained release agent and preparation method thereof.
A kind of H provided by the invention 2s sustained release agent, its raw material components by mass percentage: H 2the donor NaHS 0.5-5% of S, fruit glaze agent 1.5-15%, absolute ethyl alcohol 5-20%, paraffin 60-93%.
Its preparation method comprises the following steps:
1) NaHS and fruit glaze agent are dissolved in absolute ethyl alcohol respectively, after merging, whirlpool mixing, is prepared into mixed liquor;
2) mixed liquor is added in the paraffin of melting, ultrasonic mixing, makes the paraffin liquid containing NaHS and fruit glaze agent;
3) obtain paraffin bead by described paraffin liquid instillation cold water, through cooling, drying, obtain H 2s sustained release agent.
Wherein, described fruit glaze agent is alcohol insoluble macromolecular substance, as polyethylene glycol, lac, morpholine fatty acid salt, stearic acid etc.
Described ultrasonic power 100-500W, the time is 10-30 minute, will ensure that the temperature of mixed liquor is greater than paraffin melting point temperature in ultrasonic procedure;
Described drying mode is air drying.
H of the present invention 2s sustained release agent can in the developmental application of Promoting plant growth.Select various dose as required during use, put in the soil of planting plants, and water.
H of the present invention 2s sustained release agent has the following advantages:
1, various H is overcome 2the shortcoming that S donor rate of release is too fast;
2, product cost is low, and preparation technology is simply easy to implement;
3, H 2each composition of S sustained release agent is safe, nontoxic, meets environmental requirement;
4, slow releasing, significantly improves H 2the lasting period of S effect, reduce spraying times, reduce labour intensity.
Accompanying drawing illustrates:
Fig. 1 is the H that embodiment 1 and embodiment 2 obtain 2s sustained release agent;
Fig. 2 is the H that embodiment 1 and embodiment 2 obtain 2s sustained release agent discharges H in time in water 2the assay of S;
Fig. 3 is the growth Arabidopsis thaliana Seedlings of 2 weeks, keeps moistening after burying sustained release agent in compost, after 10 days with compare plant growth situation;
Fig. 4 is the growth Chinese cabbage seedling of 2 weeks, keeps moistening after burying sustained release agent in compost, after 10 days with compare plant growth situation.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail.
The paraffin wax (fusing point 68 DEG C) that embodiment 1. takes 10g is placed in small beaker, and heating water bath, to 70-80 DEG C, makes it fully melt; Accurately take the PEG-8000 of NaHS and 0.1g of 0.03g respectively in the centrifuge tube of two 2ml, add 1ml absolute ethyl alcohol respectively, metal bath is heated to 70-80 DEG C, makes it fully dissolve; Merged by two kinds of solution, whirlpool concussion is to fully mixing; Joined by mixed liquor in the paraffin of melting, select power 300W to make it dispersed in paraffin liquid in ultrasonic 10 minutes, this process ensures that mixeding liquid temperature is greater than 68 DEG C; Draw paraffin liquid with liquid-transfering gun, be injected into rapidly in cold water and obtain paraffin bead, cooling, pulls rear air drying out, obtains H 2s sustained release agent (see accompanying drawing 1).
The paraffin wax (fusing point 68 DEG C) that embodiment 2. takes 10g is placed in small beaker, and heating water bath, to 70-80 DEG C, makes it fully melt; Accurately take the PEG-8000 of NaHS and 0.2g of 0.05g respectively in the centrifuge tube of two 2ml, add 1ml absolute ethyl alcohol respectively, metal bath is heated to 70-80 DEG C, makes it fully dissolve; Merged by two kinds of solution, whirlpool concussion is to fully mixing; Joined by mixed liquor in the paraffin of melting, select power 300W to make it dispersed in paraffin liquid in ultrasonic 15 minutes, this process ensures that mixeding liquid temperature is greater than 68 DEG C; Draw paraffin liquid with liquid-transfering gun, be injected into rapidly in cold water and obtain paraffin bead, cooling, pulls rear air drying out, obtains H 2s sustained release agent (see accompanying drawing 1).
Bead sustained release agent prepared by Example 1 and 2 carries out release rate assay:
The preparation of working curve: accurately take 0.14gNaHS and be dissolved in 2.5ml H 2in O, obtain the NaHS mother liquor of 0.1M.Then stepwise dilution obtains NaHS final concentration is 0,1.25,2.5,5,10,20, and 40,100 μMs, get 2ml and be placed in little triangular flask with cover; Put into the Ep pipe of the 1%ZnAc being added with 500 μ L in triangular flask, room temperature places 30min; Take out the Ep pipe in little triangular flask, add DPD and FeCl of 200 μ L respectively 3, dark reaction 15min; Measure absorbance at 667nm place, obtain H 2s content standard curve: y=0.0059x-0.0005 (R 2=1).
Sustained release agent rate of release of the present invention measures: choose uniform sustained release agent bead and be placed in little triangular flask with cover respectively, add 2ml distilled water; Put into the Ep pipe of the 1%ZnAc being added with 500 μ L in triangular flask, room temperature places 30min; Take out the Ep pipe in little triangular flask, add DPD and FeCl of 200 μ L respectively 3, dark reaction 15min; Absorbance is measured at 667nm place.H is calculated according to above-mentioned calibration curve 2s content.Getting the time that sustained release agent bead stops in the with cover little triangular flask added water respectively is 1,3,5,7,10,15,20,30 days, calculate its release H 2the speed (see accompanying drawing 2) of S.
Adopt the application of above-mentioned obtained sustained release agent in different growing process:
Due to sustained release agent provided by the invention, to have in damp soil evenly, continue, stable, controllably discharge H 2the drug release feature of S, makes H 2s concentration maintains a metastable numerical value, avoids high concentration H 2the toxicity that S causes, this continual and steady administering mode adds the operability of dispenser simultaneously, more facilitates growing of plant corpus.
Sustained release agent bead 2 obtained in embodiment 3. Example 1, is placed in the growth arabidopsis culturing pot of 2 weeks, keeps the ground moistening that it covers, and after 10 days compared with the control, plant individual is obviously comparatively large, and situation of growing better (see accompanying drawing 3).
Sustained release agent bead 2 obtained in embodiment 4. Example 2, is placed in the growth Chinese cabbage culturing pot of 2 weeks, keeps the ground moistening that it covers, after 10 days compared with the control, plant individual is obviously comparatively large, and makes Chinese cabbage bloom in advance, and situation of growing better (see accompanying drawing 4).
From above result, sustained release agent provided by the invention can discharge low concentration H sustainedly and stably 2s, obvious Promoting plant growth developmental process, reaches the objects such as high yield early blossoming.

Claims (6)

1. a hydrogen sulphide sustained release agent, its raw material components by mass percentage: NaHS 0.5-5%, fruit glaze agent 1.5-15%, absolute ethyl alcohol 5-20%, paraffin 60-93%.
2. the preparation method of a kind of hydrogen sulphide sustained release agent as claimed in claim 1, is characterized in that, comprise the steps:
1) by raw material components proportioning according to claim 1, NaHS and fruit glaze agent are dissolved in absolute ethyl alcohol respectively, after merging, whirlpool mixing, is prepared into mixed liquor;
2) mixed liquor is added in the paraffin of melting, ultrasonic mixing, makes the paraffin liquid containing NaHS and fruit glaze agent;
3) obtain paraffin bead by described paraffin liquid instillation cold water, through cooling, drying, obtain hydrogen sulphide sustained release agent.
3. the preparation method of a kind of hydrogen sulphide sustained release agent as claimed in claim 2, is characterized in that, described fruit glaze agent is alcohol insoluble macromolecular substance.
4. the preparation method of a kind of hydrogen sulphide sustained release agent as claimed in claim 3, is characterized in that, described alcohol insoluble macromolecular substance is polyethylene glycol, lac, morpholine fatty acid salt or stearic acid.
5. the preparation method of a kind of hydrogen sulphide sustained release agent as claimed in claim 2, is characterized in that, described drying mode is air drying.
6. hydrogen sulphide sustained release agent as claimed in claim 1 is in the developmental application of Promoting plant growth.
CN201510217662.9A 2015-04-30 2015-04-30 A kind of hydrogen sulfide slow releasing agent and its preparation method and application Active CN104782622B (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106879627A (en) * 2017-01-24 2017-06-23 山西大学 NaHS as Plant Pollen Germination accelerator application
TWI638666B (en) 2017-03-22 2018-10-21 國立清華大學 Sustained-release composition, method for fabricating, and use thereof
CN108849978A (en) * 2018-09-07 2018-11-23 山西大学 The application as plant drought-resisting agent is used in combination in a kind of NaHS and epiphysin
CN109970162A (en) * 2019-03-28 2019-07-05 浙江大学 A kind of novel dephosphorization sustained release agent and preparation method thereof
CN113702376A (en) * 2021-08-03 2021-11-26 温州大学 Evaluation of environmental pollutants H by using zebra fish2Method of S developmental toxicity

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB568673A (en) * 1943-02-25 1945-04-16 Associated Fumigators Ltd Improvements in and relating to preparations for combating animal and insect pests
US20030235571A1 (en) * 2002-06-19 2003-12-25 Gabriel Gojon-Romanillos Systemic treatment of pathological conditions resulting from oxidative stress and/or redox imbalance
WO2013045951A1 (en) * 2011-09-30 2013-04-04 The University Of Exeter Hydrogen sulfide releasing compounds and their use
US8541396B2 (en) * 2009-04-24 2013-09-24 National University Of Singapore Morpholin-4-ium 4 methoxyphenyl (morpholino) phosphinodithioate (GYY4137) as a novel vasodilator agent
CN103734131A (en) * 2013-12-12 2014-04-23 江苏艾津农化有限责任公司 Oncomelania-hupensis killing medicament niclosamide-ethanolamine-salt sustained-release granules and preparation method thereof
WO2014132083A2 (en) * 2013-03-01 2014-09-04 Aston University Hydrogen sulphide compounds

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB568673A (en) * 1943-02-25 1945-04-16 Associated Fumigators Ltd Improvements in and relating to preparations for combating animal and insect pests
US20030235571A1 (en) * 2002-06-19 2003-12-25 Gabriel Gojon-Romanillos Systemic treatment of pathological conditions resulting from oxidative stress and/or redox imbalance
US8541396B2 (en) * 2009-04-24 2013-09-24 National University Of Singapore Morpholin-4-ium 4 methoxyphenyl (morpholino) phosphinodithioate (GYY4137) as a novel vasodilator agent
WO2013045951A1 (en) * 2011-09-30 2013-04-04 The University Of Exeter Hydrogen sulfide releasing compounds and their use
WO2014132083A2 (en) * 2013-03-01 2014-09-04 Aston University Hydrogen sulphide compounds
CN103734131A (en) * 2013-12-12 2014-04-23 江苏艾津农化有限责任公司 Oncomelania-hupensis killing medicament niclosamide-ethanolamine-salt sustained-release granules and preparation method thereof

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106879627A (en) * 2017-01-24 2017-06-23 山西大学 NaHS as Plant Pollen Germination accelerator application
CN106879627B (en) * 2017-01-24 2019-09-24 山西大学 Application of the NaHS as Plant Pollen Germination promotor
TWI638666B (en) 2017-03-22 2018-10-21 國立清華大學 Sustained-release composition, method for fabricating, and use thereof
CN108849978A (en) * 2018-09-07 2018-11-23 山西大学 The application as plant drought-resisting agent is used in combination in a kind of NaHS and epiphysin
CN109970162A (en) * 2019-03-28 2019-07-05 浙江大学 A kind of novel dephosphorization sustained release agent and preparation method thereof
CN113702376A (en) * 2021-08-03 2021-11-26 温州大学 Evaluation of environmental pollutants H by using zebra fish2Method of S developmental toxicity

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