CN106587168B - A kind of pyrite FeS2Biostimulant and preparation method thereof - Google Patents
A kind of pyrite FeS2Biostimulant and preparation method thereof Download PDFInfo
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- CN106587168B CN106587168B CN201611198522.2A CN201611198522A CN106587168B CN 106587168 B CN106587168 B CN 106587168B CN 201611198522 A CN201611198522 A CN 201611198522A CN 106587168 B CN106587168 B CN 106587168B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/12—Sulfides
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05D—INORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C; FERTILISERS PRODUCING CARBON DIOXIDE
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- C05D9/02—Other inorganic fertilisers containing trace elements
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Abstract
The invention discloses a kind of pyrite FeS2Biostimulant and preparation method thereof, by ferrous salt, many sulfate, nano heat-conductive agent, magnetized water be mixed evenly after with sodium hydrate regulator solution pH value to 9 ~ 14, after pH value has been adjusted, mixture solution is poured into stainless steel autoclave and reacted, 100 ~ 160 DEG C of controlling reaction temperature, react after 1 ~ 6h, question response kettle is naturally cooled to after room temperature, reaction product is used into deionized water successively, dilute sulfuric acid, carbon disulfide, after absolute ethyl alcohol washing for several times, product is put into vacuum drying chamber at a temperature of 105 DEG C and dried 4 hours, it is cooled to after room temperature and can obtain FeS2Product.The present invention has that preparation method is simple, conversion rate of products is high, and production cost is low, easy to operate, can rapidly prepare the pyrite FeS of high-quality2Biostimulant product, is suitable for pyrite FeS2Biostimulant industrialization large-scale production.
Description
Technical field
The invention belongs to a kind of preparation method of chemical products biostimulant, more particularly to a kind of pyrite FeS2It is biological
Stimulin and its technology of preparing.
Background technology
Pyrite (FeS2) " fool's gold " is also referred to as, there are Natural pyrite and chemical synthesis pyrite two in its source
Kind.Natural pyrite is common in the seat earth of coal seam, shale, sedimentary rock etc., is used as a kind of accessory mineral, pyrite Chang Yuhuo
Diagenesis and metamorphic rock are accompanied.Natural pyrite contains plurality of impurities, including arsenic, antimony, copper, lead, zinc, aluminium, calcium, bismuth,
Cobalt and phosphorus etc., in agriculture field, Natural pyrite can be used for providing iron for crop after Partial cleansing（Fe）And sulphur（S）'s
Fertilizer, can be used as a kind of modifying agent of basic soil.Chemical synthesis pyrite mainly has the precipitation method, vulcanization method, solvent
Hot method, hydro-thermal method.Because hydro-thermal method has simple to operate, cost is low, the characteristics of polluting small, as applying more one kind at present
Method.The pyrite of Hydrothermal Synthesiss is mainly used in lithium alloy/iron sulfide thermal cell, the pyrite application of domestic chemical synthesis
Report is there is no in the research of production estimation.There is foreign study to show, as the pyrite FeS using Hydrothermal Synthesiss2Handle farming
When species are sub-, because it can induce to form peroxide, the growth of crop can be excited.When using FeS2 (100μg/
Ml) seed of waterborne suspension pretreatment spinach, sesame and faenum graecum 12-14 hours, 60 day growth period of spinach, blade area
Index adds about 62%, and crop biomass adds 98%, and 110 days life cycle kind pod numbers of sesame improve 250%, Sesame Seed Yield
Individual plant improves 77%, and 50 day growth period lobe numbers of faenum graecum add 79%, and blade is bigger.
The pyrite of conventional hydrothermal synthesis, carries out typically all under high-temperature and high-pressure conditions, has to equipment and personal security
Certain requirement, simultaneously as being heterogeneous conditions, pyrite FeS2Conversion ratio is not high, and general only 50% or so.The present invention
Based on the deficiencies in the prior art, the pyrite technique that conventional hydrothermal is synthesized is improved, by the invention it is possible to obtain turn
The pyrite FeS of rate more than 80%2Quality product.
The content of the invention
The purpose of the present invention is in view of the shortcomings of the prior art and provides that a kind of operating condition is relatively mild, security is good,
The high pyrite FeS of reaction conversion ratio2Biostimulant and preparation method thereof.
Present invention employs following technical scheme in order to achieve the above object：
A kind of pyrite FeS2The preparation method of biostimulant comprises the following steps：
（1）Ferrous salt and many sulfate are added first after being mixed evenly in magnetized water, add nano heat-conductive agent,
Then pH=9 ~ 14 are adjusted with sodium hydroxide, obtains mixed solution；
（2）Mixed solution through step 1 is poured into stainless steel autoclave, heating response；
（3）It will be washed successively using deionized water, dilute sulfuric acid, carbon disulfide, absolute ethyl alcohol through the reacted product of step 2
Afterwards, it is put into vacuum drying chamber and dries, is subsequently cooled to after room temperature produce FeS2Biostimulant.
Further, the ferrous salt is selected from ferrous sulfate, ferrous sulfide, ferrous oxalate salt, ferrous nitrate, iron cyaniding Asia
It is one or more of in iron, frerrous chloride.
Further, many sulfate are one or more of in many sodium sulphate, many potassium sulfates.
Further, the magnetized water is that water passes through under magnetizer 3500 ~ 4500mT field strength, and magnetization is obtained for 15 ~ 18 seconds.
Further, the consumption of magnetized water described in the step 1 is thiosulfate and the 5-10 of ferrous salt gross mass
Times, wherein ferrous salt：Thiosulfate mol ratio is 1:(1~10).
Further, the nano heat-conductive agent addition is ferrous salt and ‰ ~ 5wt of 1wt ‰ of thiosulfate gross mass.
Further, the nano heat-conductive agent is CNT, copper nanoparticle.
Further, heating response condition is in the step 2：100 ~ 160 DEG C of reaction temperature, 1 ~ 6h of reaction time.
Further, condition is dried in vacuo in the step 2 is：Dried 4 hours at a temperature of 105 DEG C.
Compared with prior art, the device have the advantages that：
1st, the present invention have selected the nano heat-conductive agent such as CNT, copper nanoparticle and participate in ferrous salt compound and many sulfate
The hydrothermal synthesis reaction of compound, due to nano heat-conductive agent, it has the effect of hydrothermal reaction process hot-fluid energy of exciting, can be with
The effective reaction heat provided needed for Hydrothermal Synthesiss, so as to be conducive to improving pyrite FeS2Reaction conversion ratio, simultaneously because
Its addition is few, to pyrite FeS2Production cost influence it is little, be suitable for industrial-scale expanding production.
2nd, magnetized water has relatively low surface tension, relative to common deionized water, to ferrous salt compound and many sulfuric acid
Salt compound has more preferable solvability, is conducive to eliminating the influence that conventional hydrothermal synthesizes heterogeneous reaction, so as to promote Asia
Molysite compound and the reaction of many sulphate cpds are preferably carried out, and improve the conversion ratio of target product.
3rd, the present invention excites hydro-thermal anti-due to having used CNT, copper nanoparticle etc. as thermal conducting agent because it has
The effect of process hot-fluid energy is answered, lower is required to reactor HTHP, therefore, relatively mild with operating condition, safety
The features such as property is good.
Embodiment
The present invention is specifically described below by embodiment, it is necessary to it is pointed out here that be that the present embodiment is served only for pair
The present invention is further described, but it is not intended that limiting the scope of the invention.The person skilled in the art in the field
Some nonessential modifications and adaptations can be made according to the content of the invention described above.
Embodiment 1
Pyrite FeS2The preparation of biostimulant：
First by 1.5g ferrous sulfate, 6.23g sodium thiosulfate Na2S2O3, account for ferrous sulfate and sodium thiosulfate Na2S2O3
The 3wt ‰ of gross mass CNT adds 77.3g magnetized water（By under magnetizer 3500 ~ 4500mT field strength, magnetizing 15 ~ 18
Second obtains）In stir, obtain the mixed solution of three, adjust pH=11 with sodium hydroxide, then mixed solution poured into stainless
In steel autoclave, 120 DEG C of heating response 3h obtain pyrite FeS2Coarse products.Then by obtained coarse products successively
After being washed with deionized water, dilute sulfuric acid, carbon disulfide, absolute ethyl alcohol, dry 4 are put into vacuum drying chamber at a temperature of 105 DEG C small
When, it is finally cooled to after room temperature can obtain FeS of the present invention2Biostimulant target product, measures FeS2Conversion ratio 82.2%.
Comparative example 1a：
First by 1.5g ferrous sulfate, 6.23g sodium thiosulfate Na2S2O3Add and stirred in 77.3g deionized waters,
Mixed solution is obtained, pH=11 are adjusted with sodium hydroxide, then mixed solution is poured into stainless steel autoclave, 120 DEG C of heating
Reaction 3h obtains pyrite FeS2Coarse products.Then obtained coarse products are used into deionized water, dilute sulfuric acid, curing successively
After carbon, absolute ethyl alcohol washing, it is put into vacuum drying chamber at a temperature of 105 DEG C and dries 4 hours, be finally cooled to after room temperature to obtain
To FeS2Biostimulant, measures FeS2Conversion ratio 45.17%.
Comparative example 1b：
First by 1.5g ferrous sulfate, 6.23g sodium thiosulfate Na2S2O3Add 77.3g magnetized water（By magnetizer
Under 3500 ~ 4500mT field strength, magnetization is obtained for 15 ~ 18 seconds）In stir, obtain mixed solution, with sodium hydroxide adjust pH=
11, then mixed solution is poured into stainless steel autoclave, 120 DEG C of heating response 3h obtain pyrite FeS2Coarse products.
Then after obtained coarse products are washed with deionized water, dilute sulfuric acid, carbon disulfide, absolute ethyl alcohol successively, it is put into vacuum and does
Dried 4 hours at a temperature of 105 DEG C in dry case, be finally cooled to after room temperature can obtain FeS2Biostimulant, measures FeS2Conversion
Rate 51.23%.
Conclusion：
Comparative example 1a instead of magnetized water with deionized water compared to embodiment 1, and without CNT, final
To FeS2 conversion ratios be only 45.17%.
Comparative example 1b adds magnetized water on the basis of comparative example 1a, the FeS finally given2Conversion ratio is than comparative example 1a
It is slightly higher, it is 51.23%, it is seen that because the low surface tension of magnetized water is acted on, ferrous sulfate, sodium thiosulfate Na2S2O3In reaction
Under the hot conditions of kettle, solubility is more preferable, so as to be conducive to FeS to a certain extent2Conversion, improves FeS2Conversion ratio.
Embodiment 1 adds CNT under the conditions of magnetized water, its FeS2Conversion ratio rises to 82.2%, it can be seen that,
The effect of the present invention is better than comparative example 1a and 1b, illustrates that magnetized water and CNT in the present invention have played Synergistic work
With obtaining more preferably FeS2Conversion ratio.
Embodiment 2
Pyrite FeS2The preparation of biostimulant：
First by 1.6g ferrous sulfides, 2.7g potassium thiosulfates K2S2O3, account for ferrous sulfide and potassium thiosulfate K2S2O3Always
The 1wt ‰ of quality CNT adds 43g magnetized water（By under magnetizer 3500 ~ 4500mT field strength, magnetization is obtained for 15 ~ 18 seconds
Arrive）In stir, obtain the mixed solution of three, with sodium hydroxide adjust pH=10, mixed solution is poured into stainless steel high pressure
In reactor, 160 DEG C of heating response 4h obtain pyrite FeS2Coarse products.Then by obtained coarse products spend successively from
After sub- water, dilute sulfuric acid, carbon disulfide, absolute ethyl alcohol washing, drying 4 hours at a temperature of 105 DEG C are put into vacuum drying chamber, finally
It is cooled to after room temperature and can obtain FeS of the present invention2Biostimulant target product, FeS2Conversion ratio 81.7%.
Comparative example 2a
First by 1.6g ferrous sulfides, 2.7g potassium thiosulfates K2S2O3Add and stirred in 43g deionized waters, obtained
Mixed solution, adjusts pH=10 with sodium hydroxide, mixed solution is poured into stainless steel autoclave, 160 DEG C of heating response 4h
Obtain pyrite FeS2Coarse products.Then obtained coarse products are used into deionized water, dilute sulfuric acid, carbon disulfide, nothing successively
After water-ethanol washing, it is put into vacuum drying chamber at a temperature of 105 DEG C and dries 4 hours, is finally cooled to after room temperature can obtain
FeS2Biostimulant, FeS2Conversion ratio 50.86%.
Comparative example 2b
First by 1.6g ferrous sulfides, 2.7g potassium thiosulfates K2S2O3Add 43g magnetized water（By magnetizer 3500 ~
Under 4500mT field strength, magnetization is obtained for 15 ~ 18 seconds）In stir, obtain mixed solution, pH=10 adjusted with sodium hydroxide, will be mixed
Close solution to pour into stainless steel autoclave, 160 DEG C of heating response 4h obtain pyrite FeS2Coarse products.Then it will obtain
Coarse products washed successively with deionized water, dilute sulfuric acid, carbon disulfide, absolute ethyl alcohol after, be put into vacuum drying chamber 105 DEG C
At a temperature of dry 4 hours, be finally cooled to after room temperature can obtain FeS2Biostimulant, FeS2Conversion ratio 54.21%.
Conclusion：
Comparative example 2a instead of magnetized water with deionized water compared to embodiment 2, and without CNT, final
The FeS arrived2Conversion ratio is only 50.86%.
Comparative example 2b adds magnetized water on the basis of comparative example 2a, the FeS finally given2Conversion ratio is than comparative example 2a
It is slightly higher, it is 54.21%, it is seen that because the low surface tension of magnetized water is acted on, ferrous sulfide, potassium thiosulfate K2S2O3In reactor
Hot conditions under, solubility more preferably, so as to be conducive to FeS to a certain extent2Conversion, improves FeS2 conversion ratios.
Embodiment 2 adds CNT under the conditions of magnetized water, its FeS2Conversion ratio rises to 81.7%, it can be seen that,
The effect of the present invention is better than comparative example 2a and 2b, illustrates that magnetized water and CNT in the present invention have played Synergistic work
With obtaining more preferably FeS2Conversion ratio.
Embodiment 3
Pyrite FeS2The preparation of biostimulant：
First by 1.8g ferrous sulfides, 3.4g potassium thiosulfates K2S2O3, account for ferrous sulfide and potassium thiosulfate K2S2O3Always
The 2.6wt ‰ of quality copper nanoparticle adds 52g magnetized water（By under magnetizer 3500 ~ 4500mT field strength, magnetizing 15 ~ 18 seconds
Obtain）In stir, obtain the mixed solution of three, pH=12 adjusted with sodium hydroxide, it is high that mixed solution is poured into stainless steel
Press in reactor, 130 DEG C of heating response 3h obtain pyrite FeS2Coarse products.Then obtained coarse products are spent successively
After ionized water, dilute sulfuric acid, carbon disulfide, absolute ethyl alcohol washing, drying 4 hours at a temperature of 105 DEG C are put into vacuum drying chamber, most
After be cooled to after room temperature and can obtain FeS of the present invention2Biostimulant target product, FeS2Conversion ratio 84.6%.
Comparative example 3a
First by 1.8g ferrous sulfides, 3.4g potassium thiosulfates K2S2O3Add and stirred in 52g deionized waters, obtained
Mixed solution, adjusts pH=12 with sodium hydroxide, mixed solution is poured into stainless steel autoclave, 130 DEG C of heating response 3h
Obtain pyrite FeS2Coarse products.Then obtained coarse products are used into deionized water, dilute sulfuric acid, carbon disulfide, nothing successively
After water-ethanol washing, it is put into vacuum drying chamber at a temperature of 105 DEG C and dries 4 hours, is finally cooled to after room temperature can obtain
FeS2Biostimulant, FeS2Conversion ratio 48.63%.
Comparative example 3b
First by 1.8g ferrous sulfides, 3.4g potassium thiosulfates K2S2O3Add 52g demagnetization water（By magnetizer 3500 ~
Under 4500mT field strength, magnetization is obtained for 15 ~ 18 seconds）In stir, obtain mixed solution, pH=12 adjusted with sodium hydroxide, will be mixed
Close solution to pour into stainless steel autoclave, 130 DEG C of heating response 3h obtain pyrite FeS2Coarse products.Then it will obtain
Coarse products washed successively with deionized water, dilute sulfuric acid, carbon disulfide, absolute ethyl alcohol after, be put into vacuum drying chamber 105 DEG C
At a temperature of dry 4 hours, be finally cooled to after room temperature can obtain FeS2Biostimulant, FeS2Conversion ratio 52.34%.
Conclusion：
Comparative example 3a instead of magnetized water with deionized water compared to embodiment 3, and without CNT, final
The FeS arrived2Conversion ratio is only 48.63%.
Comparative example 3b adds magnetized water on the basis of comparative example 3a, the FeS finally given2Conversion ratio is than comparative example 3a
It is slightly higher, it is 52.34%, it is seen that because the low surface tension of magnetized water is acted on, ferrous sulfide, potassium thiosulfate K2S2O3In reactor
Hot conditions under, solubility more preferably, so as to be conducive to FeS to a certain extent2Conversion, improves FeS2 conversion ratios.
Embodiment 3 adds copper nanoparticle under the conditions of magnetized water, its FeS2Conversion ratio rises to 84.6%, it can be seen that,
The effect of the present invention is better than comparative example 3a and 3b, illustrates that the magnetized water in the present invention and copper nanoparticle have played Synergistic work
With obtaining more preferably FeS2Conversion ratio.
Claims (8)
1. a kind of pyrite FeS2The preparation method of biostimulant, it is characterised in that：The preparation method comprises the following steps：
（1）Ferrous salt and many sulfate are added first after being mixed evenly in magnetized water, add nano heat-conductive agent, then
PH=9 ~ 14 are adjusted with sodium hydroxide, mixed solution is obtained；
（2）Will be through step（1）Mixed solution pour into stainless steel autoclave, heating response；Reaction temperature 100 ~ 160
DEG C, 1 ~ 6h of reaction time；
（3）Will be through step（2）Reacted product is successively using deionized water, dilute sulfuric acid, carbon disulfide, absolute ethyl alcohol washing
Afterwards, it is put into vacuum drying chamber and dries, is subsequently cooled to after room temperature produce FeS2Biostimulant.
2. pyrite FeS according to claim 12The preparation method of biostimulant, it is characterised in that：The ferrous salt
It is one or more of in ferrous sulfate, ferrous sulfide, ferrous oxalate, ferrous nitrate, ferroferricyanide, frerrous chloride.
3. pyrite FeS according to claim 12The preparation method of biostimulant, it is characterised in that：Many sulfuric acid
Salt is one or more of in many sodium sulphate, many potassium sulfates.
4. pyrite FeS according to claim 12The preparation method of biostimulant, it is characterised in that：The magnetized water
Pass through for water under magnetizer 3500 ~ 4500mT field strength, magnetization is obtained for 15 ~ 18 seconds.
5. the pyrite FeS according to claim 1 or 42The preparation method of biostimulant, it is characterised in that：Step（1）
In many sulfate be selected from thiosulfate, the consumption of the magnetized water is thiosulfate and the 5-10 of ferrous salt gross mass
Times, wherein ferrous salt：Thiosulfate mol ratio is 1:(1~10).
6. pyrite FeS according to claim 12The preparation method of biostimulant, it is characterised in that：Step（1）In
Many sulfate are selected from thiosulfate, the nano heat-conductive agent addition be ferrous salt and thiosulfate gross mass 1wt ‰ ~
5wt‰。
7. pyrite FeS according to claim 62The preparation method of biostimulant, it is characterised in that：The nanometer is led
Thermit powder is CNT, copper nanoparticle.
8. pyrite FeS according to claim 12The preparation method of biostimulant, it is characterised in that：The step（3）
Middle vacuum drying condition is：Dried 4 hours at a temperature of 105 DEG C.
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| CN112197262B (en) * | 2020-10-24 | 2023-06-27 | 四川泸天化创新研究院有限公司 | Intelligent control method for circulating fluidized bed coal-fired boiler |
| CN114853146B (en) * | 2022-04-25 | 2023-10-31 | 武汉理工大学 | Water treatment agent and water treatment method for magnetic recyclable pyrite catalyst |
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