CN102531772A - Method for preparing organic titanium-plant vinegar ammonium salt organic fertilizer - Google Patents
Method for preparing organic titanium-plant vinegar ammonium salt organic fertilizer Download PDFInfo
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Abstract
The invention relates to a method for preparing organic titanium-plant vinegar ammonium salt organic fertilizer. The method is characterized in that new sediment metatitanic acid is prepared by using alkali to neutralize ice water solution of titanium salt; the metatitanic acid is used to replace titanic chloride and sulfate as raw materials for the synthesis of citricacide-titatnium chelate; the new sediment metatitanic acid is used as a titanium source, the citric acid is used as acid solvent and chelant, and a microwave hot melting chelate technology is used to synthesize the citricacide-titatnium chelate; and then the saturated solution of citricacide-titatnium chelate is subjected to neutralization and salting-out by the alkaline plant vinegar composite ammonium to prepare the organic titanium-plant vinegar ammonium salt organic fertilizer. The citricacide-titatnium chelate prepared by the microwave hot melting chelate technology with excellent stability and water solubility is used as synergist of plant vinegar ammonium organic fertilizer and crop growth promoter.
Description
Technical field
The invention belongs to technical field of fertilizers, be specifically related to a kind of by organic titanium-the plant method of manufacture of vinegar ammonium salt fertilizer.
Background technology
Fertilizer is the strategic materials that ensure national food safety, keeps and increase fertility of land realizing the basic substance of agricultural sustainable development.
Chemical fertilizer is still the important production means of present agriculture prodn; Plant is very low to the chemical fertilizer absorption rate in the soil; According to China's comprehensive scientific and technological level determination of agricultural at present; The utilization ratio of China's agricultural crops fertilising is merely about 30%, causes the pollution of a large amount of fertilizer loss wastes and environment.
The new-type fertilizer research and development of high-absorbility are the technological innovation focuses of current technical field of fertilizers; Countries in the world to the low problem of chemical fertilizer absorption rate in the soil, have been dropped into great amount of manpower and material resources, the new-type fertilizer of research and development high-absorbility energetically to plant.
Titanium elements is described as " catalyzer of fertilizer ", and it can promote plant to nitrogen, phosphorus, potassium and other moderate-element, trace elements absorbed and running forcefully.Use the compound manure that contains titanium elements and both can reach additional plant nutrition, can greatly promote absorption and the utilization of plant again nutritive ingredient.
According to domestic and international research department the test-results of using the compound manure that contains organic titanium is shown: use the compound manure that contains organic titanium; Can be on the level of original plant to the fertilizer absorption rate; Improve absorption rate 20% ~ 30%, the compound manure that contains organic titanium is a kind of new-type fertilizer of high utilization rate.
Titanium elements still is a kind of very effective non-hormone plant-growth regulator:
Titanium elements can improve photosynthesis of plants, increases the chlorophyll content in the plant leaf;
The activity of plurality of enzymes (like px, katalase, nitrogenase, nitrate reductase, 2-6 Phosphoric acid esterase etc.) in the titanium elements ability activated plant body;
Titanium elements can promote to improve the resistance of crop, and strengthening immunity is significantly improved to the ability of the drought resisting of crop, waterlogging-resistant, cold-resistant, high temperature resistance, disease and insect resistance;
Titanium elements can promote crop precocious, increases agricultural output;
Titanium elements can improve the quality of agricultural-food, improves the content of various nutritive ingredients in the agricultural-food, reduces the odd fruit rate, makes fruit shape plentiful, lovely luster.
The compound manure that contains organic titanium is that trace element fertilizer is formed by water miscible organic titanium inner complex and common nitrogen, phosphorus, potassic fertilizer and other secondary nutrientses, is the new type functional fertilizer of a kind of plant nutrition and physiological regulation economic benefits and social benefits unification.
The use of the compound manure of organic titanium on farm crop do not receive area, soil and weather condition effect, is a kind of broad spectrum that is applicable to Different Crop, the functional fertilizer that consumption is low.
Patent documentation CN1052302A discloses the patented technology with titanium tetrachloride and the synthetic plant growth regulator of Hydrocerol A;
Patent documentation CN101838159A discloses the patented technology that contains the functional fertilizer of titanium complex with preparations such as titanium sulfate and tartrate, Hydrocerol A, oxysuccinic acid, mandelic acid, lactic acid.
Above patent documentation discloses direct muriate with water-soluble titanium; Or the vitriol of titanium is as the raw material of synthesizing citric acid organic titanium inner complex, and the weak point of its existence is will mix with a large amount of cl ionss or sulfonium ion in institute's synthetic Hydrocerol A organic titanium inner complex.
Planting vinegar is to form fluent meterial by vegetable materials such as timber, shell, bamboo wood, stalk, husk and the condensation of industrial wood waste pyrolytic gasification thing thereof, and its staple is crude substance such as organic acid, phenols, ketone, aldehydes, alcohols and heterocyclic.
Plant in the vinegar by what timber, shell were processed and be wooden vinegar; By bamboo wood process for bamboo vinegar; By stalk, husk process for careless vinegar (claiming stalk vinegar again).Plant that vinegar can be used as organic pesticide (sterilant, Insecticides (tech) & Herbicides (tech)) and fertilizer in Organic farming, soil improvement agent uses.
Plant in the organic fertilizer that vinegar forms and have the intensive seepage force owing to plant the vinegar composition; Can improve fertilizer efficiency 30% ~ 50%; Plant vinegar simultaneously and can also improve the function of stress resistance of plant, to the diseases prevention of crop, antibiotic, expelling parasite has effect preferably, is a kind of multi-functional organic fertilizer.
But plant vinegar fertilizer double as soil conditioner again, can promote the growth of aerobic bacteria in the soil, suppress the harmful microbe breeding; Be released in the nutritive element that is cured in the soil, also can improve the soil microorganisms structure again, reduce the generation of soil source disease effectively; To solving soil continuous cropping obstacle effect is preferably arranged, and can alleviate the soil salinization, inferior degree of salinity, play the effect of regulating soil pH value; Promote plant root system development, improve the transplanting success of plant.
Plant the vinegar ammonium salt compound and be by wooden vinegar or bamboo vinegar or careless vinegar and alkaline ammonium salt such as volatile salt, volatile caustic and carry out acid-base reaction and generate.
Planting the vinegar ammonium salt compound is a kind of novel organic ammonium salt, and it has possessed the advantage and the effect of all inorganic nitrogenous fertilizers, and having both has additional nitrogen and plant the organotrophic double effects of vinegar.Planting the vinegar ammonium salt compound compares with inorganic nitrogenous fertilizers such as traditional ammonium chloride, ammonium sulfate; There are not sulfate radical and cl ions residual in soil; Can not cause the acidifying of soil to harden; Eliminated traditional nitrogenous fertilizer such as ammonium chloride, ammonium sulfate and made the restrictive factor of amount, also can not cause the decline of yam, beet, quality of tobacco in raising.Plant the vinegar ammonium salt compound simultaneously and have the function that significantly improves crop anti-adversity, the obvious enhancing crop of ability is cold-resistant, the ability of disease and insect resistance.
Patent documentation CN1225983C discloses the patented technology of the wooden vinegar multi-effect plant growth promotor of being made up of wooden vinegar, urea, potassium primary phosphate, humic acids, Hydrocerol A, lactic acid, boric acid, ammonium molybdate, zinc sulfate, manganous sulfate, copper sulfate, ferrous sulfate, sal epsom, disodium salt etc.;
Patent documentation CN100421562C disclose have coordinate plant growth and necessarily antibacterial, sterilization, the bamboo vinegar of anthelminthic effect is matrix, adds the protectant patented technology of bamboo vinegar liquid plant nutrition that urea, potassium primary phosphate, saltpetre, sal epsom, ferrous sulfate, manganous sulfate, zinc sulfate, copper sulfate, borax, ammonium molybdate etc. are formed;
It is matrix that patent documentation CN100364934C discloses with wood (grass) vinegar liquid, adds the patented technology of wood (grass) the vinegar liquid fertilizer of compositions such as urea, potassium primary phosphate, saltpetre, nitrocalcite, sal epsom, ferrous sulfate, manganous sulfate, zinc sulfate, copper sulfate, borax or boric acid, Sodium orthomolybdate or ammonium molybdate and REE, humic acids;
Patent documentation CN101176474A discloses by bamboo vinegar, wooden vinegar or careless vinegar liquid and traditional chemical herbicide and has formed biogenic steriland herbicide, and has both the promotion plant-growth, the patented technology of the effect of improving the soil;
Patent documentation CN101263810A discloses by planting vinegar and inert ingredient, macroelement, trace element, sequestrant etc. and has formed the patented technology of pesticides antidote;
It is main that patent documentation CN101606536A discloses by wood vinegar, the patented technology of the soil disinfectant of forming with copper sulfate, ferrous sulfate, avermitilis strain etc.;
Patent documentation CN1647635A discloses with quicklime (unslaked lime) and has handled the patented technology that bamboo vinegar liquid prepares bamboo vinegar liquid compound salt preservative and freshness keeping agent;
Patent documentation CN100368509C discloses the patented technology that has multifunction green farmingization products such as supplying with full nutrition, coordinate plant growth growth, bactericidal and disinfest with the preparation of alkaline matter for processing plant vinegar liquid;
The below disclosed patent of planting vinegar (wooden vinegar, bamboo vinegar, careless vinegar) liquid that relates to has been applied to upward fields such as weedicide, pesticides antidote, soil disinfectant, antisepsis antistaling agent and multifunctional green farmingization product of plant growth promoter, plant nutrition protective material, liquid fertilizer and agricultural.
Through retrieving disclosed patent documentation and memoir:
Find to be employed in the frozen water with the report for preparing the metatitanic acid that can be dissolved in Hydrocerol A in the alkalescence with titanium salt; Do not find with the report of new deposition metatitanic acid as the titanium source of preparation lemon titanium; Do not find report with microwave hot melt chelating technology synthesizing citric acid titanium.
Through retrieving disclosed patent documentation and memoir:
Do not find by the report of organic titanium with the multifunctional organic fertilizer of planting the combination of vinegar composite salt; Do not find with alkalescence (pH >=8) plant the vinegar ammonium salt compound as analysing the salt neutralizing agent, preparation organic titanium-the plant report of vinegar ammonium salt compound multifunctional fertilizers of saltouing neutralizes.
Summary of the invention
One of the object of the invention provides a kind of method of manufacture of Hydrocerol A titanium of not chloride, sulfonium ion;
Two of the object of the invention provides a kind of organic titanium of not chloride, sulfonium ion-the plant method of manufacture of vinegar ammonium salt compound multifunctional organic fertilizer.
The object of the invention is realized through following technical scheme: the present invention is a kind of usefulness prepared organic titanium-plant method of vinegar ammonium salt multifunctional organic fertilizer material of saltouing; It is characterized in that: with in the alkali with a kind of not chloride, sulfonium ion of frozen water formulations prepared from solutions of titanium salt, can be dissolved in the new deposition metatitanic acid of Hydrocerol A; With not chloride, sulfonium ion, can be dissolved in the new deposition metatitanic acid of Hydrocerol A, the muriate of instead of titanium, vitriol are as the raw material of the Hydrocerol A titanium of synthetic not chloride, sulfonium ion; With not chloride, sulfonium ion, the new deposition metatitanic acid that can be dissolved in Hydrocerol A is the titanium source, is sour solvent, sequestrant with Hydrocerol A, synthesizes Hydrocerol A titanium not chloride, sulfonium ion with microwave hot melt chelating technology; Hydrocerol A titanium saturated solution is planted the compound ammonium of vinegar neutralization preparation organic titanium-the plant vinegar ammonium salt fertilizer of saltouing with alkalescence.
Described with in the alkali with the frozen water solution of titanium salt, the new deposition metatitanic acid of preparation, preparation according to the following steps:
A, the vitriol of the muriate of titanium or titanium is dissolved among the frozen water, with the neutralization of 10% ~ 30% sodium hydroxide solution, control pH is 7.0 ~ 8.0, and deposition is separated out oyster white gel metatitanic acid in≤5 ℃ cold water;
B, new sedimentary metatitanic acid are removed cl ions or sulfonium ion with distilled water wash;
After the new sedimentary metatitanic acid of c, washing removal cl ions or sulfonium ion removes the part planar water with whizzer, in time be used for acid and dissolve chelating.
Described new deposition metatitanic acid and Hydrocerol A are in the ratio proportioning of titanium: Hydrocerol A=1:2.5 ~ 4 mol ratios.
Described with microwave hot melt chelating technology according to the following steps:
The preparation of a, Hydrocerol A-metatitanic acid suspension mixed solution:
In titanium: the ratio proportioning of the mol ratio 1:2.5 of Hydrocerol A ~ 4, the Citric acid monohydrate Food grade of xln is dissolved in the planar water of new deposition metatitanic acid, stirring generates milky Hydrocerol A-metatitanic acid suspension mixed solution;
B, microwave hot melt chelating technology synthesizing citric acid titanium:
Hydrocerol A-metatitanic acid suspension mixed solution is placed in the special disc type teflon resin reaction vessel; With operating frequency 915MHz or use operating frequency 2450MHz; The cabinet type microwave device of microwave power 1 ~ 10KW; Or tunnel type micro wave equipment carries out radiation hot melt chelating, and the microwave thermal melting temperatur is controlled at 100 ℃ ~ 120 ℃, and reaction end is that milky suspension mixed solution becomes water white glue;
The preparation of c, Hydrocerol A titanium saturated solution:
Hydrocerol A titanium glue with microwave hot melt chelating is processed when glue also is in the hot melt state, becomes Hydrocerol A titanium saturated solution with distilled water diluting.
Described Hydrocerol A titanium saturated solution is saltoutd technology according to the following steps with the vinegar ammonium salt of planting of alkalescence:
A, alkalescence are planted the preparation of vinegar ammonium salt compound:
To plant vinegar (containing wooden vinegar, bamboo vinegar, careless vinegar), to use volatile salt or solution of ammonium hydroxide to regulate pH be 8.0 ~ 12.0, and clarification filtration is removed materials such as tar, benzopyrene, filtrates and plant the vinegar ammonium salt compound for alkalescence;
B, acid Hydrocerol A titanium-the plant preparation of vinegar ammonium salt compound:
Hydrocerol A titanium saturated solution is regulated pH to 1.5 ~ 2.5 with the vinegar ammonium salt compound of planting of alkalescence; Make the Hydrocerol A titanium and plant the vinegar ammonium salt compound and form the gel object and separate out; Ageing is after 24 hours in≤25 ℃ of room temperatures; Remove surface adsorption water at 60 ℃ of hot blasts, be the acid Hydrocerol A titanium of leather hard-the plant composite salt of vinegar ammonium salt compound;
C, organic titanium-the plant preparation of vinegar ammonium salt compound multifunctional organic fertilizer:
With the Hydrocerol A titanium of leather hard-plant vinegar ammonium salt compound and Carbon Dioxide ammonium proportional mixing, finally controlling its pH is 5.5 ~ 6.5, and organic titanium-plant vinegar ammonium salt compound multifunctional organic fertilizer material is processed in oven dry in 60 ℃ ± 5 ℃ baking oven.
Technology of the present invention is to directly with the vitriol of the muriate of titanium or the titanium raw material as the synthesizing citric acid titanium; Can make in institute's synthetic organic titanium to mix the defective that cl ions or sulfonium ion are arranged, propose to synthesize the raw material of organic titanium with metatitanic acid conduct not chloride, sulfonium ion.
Compare with prior art; Stable superior, the water miscible Hydrocerol A titanium that the present invention will be processed by the abundant chelating of microwave hot melt is as synergistic agent and the plant growth promotor that plant vinegar ammonium fertilizer, and the various activity of various activity and organic titanium that will plant the vinegar fertilizer are superimposed.
Embodiment
Below in conjunction with embodiment the present invention is elaborated, but do not limit the scope of the present invention.
Embodiment 1
(1) preparation of metatitanic acid:
A, in the beaker of 1500ml, add 0 ℃ ~ 5 ℃ the frozen water of 1000ml; Under the stirring of electric mixer, be added dropwise to 10ml hydrochloric acid and 20ml titanium tetrachloride, generate the titanium tetrachloride hydrochloric acid soln; With in 10% the sodium hydroxide solution with the titanium tetrachloride hydrochloric acid soln; Control solution temperature≤5 ℃, pH value 7.0 ~ 8.0 precipitates metatitanic acid and separates out in≤5 ℃ cold water;
B, new sedimentary metatitanic acid are removed cl ions with distilled water wash;
After the metatitanic acid of c, washing removal cl ions removes the part planar water with whizzer, promptly can be used for acid and dissolve chelating.
(2) preparation of Hydrocerol A titanium chelate:
The preparation of a, Hydrocerol A-metatitanic acid suspension mixed solution:
Titaniferous is 8.7g in the prepared metatitanic acid of the titanium tetrachloride of 20ml; In titanium: the ratio proportioning of the mol ratio 1:3 of Hydrocerol A; Add Citric acid monohydrate Food grade crystallization powder 115g at metatitanic acid; Be stirred in the planar water that solid citric acid is dissolved in metatitanic acid with electric mixer, form Hydrocerol A-metatitanic acid suspended mixture;
B, microwave hot melt chelating technology synthesizing citric acid titanium:
Hydrocerol A-metatitanic acid suspension mixed solution is placed in the special disc type teflon resin reaction vessel; With cabinet type microwave stove hot melt chelating under 100 ℃ ~ 120 ℃ temperature of 2450MHz frequency 1000W, reaction end is that milky suspension mixed solution becomes water white glue;
The preparation of c, Hydrocerol A titanium saturated solution:
Hydrocerol A titanium glue with microwave hot melt chelating is processed becomes Hydrocerol A titanium saturated solution with distilled water diluting when glue is in the hot melt state.
(3) with prepared organic titanium-the plant method of vinegar ammonium salt multifunctional organic fertilizer material of saltouing:
A, alkalescence are planted the preparation of vinegar ammonium salt compound:
To plant vinegar (containing wooden vinegar, bamboo vinegar, careless vinegar), to use volatile salt or solution of ammonium hydroxide to regulate pH be 8.0 ~ 12.0, and clarification filtration is removed materials such as tar, benzopyrene, filtrates and plant the vinegar ammonium salt compound for alkalescence;
B, acid Hydrocerol A titanium-the plant preparation of vinegar ammonium salt compound:
Hydrocerol A titanium saturated solution is regulated pH to 1.5 ~ 2.5 with the vinegar ammonium salt compound of planting of alkalescence; Make the Hydrocerol A titanium and plant the vinegar ammonium salt compound and form the gel object and separate out; Ageing is after 24 hours in≤25 ℃ of room temperatures; Remove surface adsorption water at 60 ℃ of hot blasts, be the acid Hydrocerol A titanium of leather hard-the plant composite salt of vinegar ammonium salt compound
C, organic titanium-the plant preparation of vinegar ammonium salt compound multifunctional organic fertilizer:
With leather hard the Hydrocerol A titanium-planting the vinegar ammonium salt compound mixes with the part by weight of Carbon Dioxide ammonium by 1.0:1.0, finally controlling its pH is 5.5 ~ 6.5, organic titanium-plant vinegar ammonium salt compound multifunctional organic fertilizer material is processed in oven dry in 60 ℃ ± 5 ℃ baking oven.
Embodiment 2
(1) preparation of metatitanic acid:
A, in the beaker of 1500ml, add 0 ℃ ~ 5 ℃ the frozen water of 1000ml; Under the stirring of electric mixer, be added dropwise to 10ml hydrochloric acid and 20ml titanium tetrachloride, generate the titanium tetrachloride hydrochloric acid soln; With in 10% the sodium hydroxide solution with the titanium tetrachloride hydrochloric acid soln; Control solution temperature≤5 ℃, pH value 7.0 ~ 8.0 precipitates metatitanic acid and separates out in≤5 ℃ cold water;
B, new sedimentary metatitanic acid are removed cl ions with distilled water wash;
After the metatitanic acid of c, washing removal cl ions removes the part planar water with whizzer, promptly can be used for acid and dissolve chelating.
(2) preparation of Hydrocerol A titanium chelate:
The preparation of a, Hydrocerol A-metatitanic acid suspension mixed solution:
Titaniferous is 8.7g in the prepared metatitanic acid of the titanium tetrachloride of 20ml; In titanium: the ratio proportioning of the mol ratio 1:2.5 of Hydrocerol A; Add Citric acid monohydrate Food grade crystallization powder 96g at metatitanic acid; Be stirred in the planar water that solid citric acid is dissolved in metatitanic acid with electric mixer, form Hydrocerol A-metatitanic acid suspended mixture;
B, microwave hot melt chelating technology synthesizing citric acid titanium:
Hydrocerol A-metatitanic acid suspension mixed solution is placed in the special disc type teflon resin reaction vessel; With cabinet type microwave stove hot melt chelating under 100 ℃ ~ 120 ℃ temperature of 2450MHz frequency 1000W, reaction end is that milky suspension mixed solution becomes water white glue;
The preparation of c, Hydrocerol A titanium saturated solution:
Hydrocerol A titanium glue with microwave hot melt chelating is processed becomes Hydrocerol A titanium saturated solution with distilled water diluting when glue is in the hot melt state.
(3) with prepared organic titanium-the plant method of vinegar ammonium salt multifunctional organic fertilizer material of saltouing:
A, alkalescence are planted the preparation of vinegar ammonium salt compound:
To plant vinegar (containing wooden vinegar, bamboo vinegar, careless vinegar), to use volatile salt or solution of ammonium hydroxide to regulate pH be 8.0 ~ 12.0, and clarification filtration is removed materials such as tar, benzopyrene, filtrates and plant the vinegar ammonium salt compound for alkalescence;
B, acid Hydrocerol A titanium-the plant preparation of vinegar ammonium salt compound:
Hydrocerol A titanium saturated solution is regulated pH to 1.5 ~ 2.5 with the vinegar ammonium salt compound of planting of alkalescence; Make the Hydrocerol A titanium and plant the vinegar ammonium salt compound and form the gel object and separate out; Ageing is after 24 hours in≤25 ℃ of room temperatures; Remove surface adsorption water at 60 ℃ of hot blasts, be the acid Hydrocerol A titanium of leather hard-the plant composite salt of vinegar ammonium salt compound
C, organic titanium-the plant preparation of vinegar ammonium salt compound multifunctional organic fertilizer:
With leather hard the Hydrocerol A titanium-planting the vinegar ammonium salt compound mixes with the part by weight of Carbon Dioxide ammonium by 1.0:0.8, finally controlling its pH is 5.5 ~ 6.5, organic titanium-plant vinegar ammonium salt compound multifunctional organic fertilizer material is processed in oven dry in 60 ℃ ± 5 ℃ baking oven.
Embodiment 3
(1) preparation of metatitanic acid:
A, in the beaker of 1500ml, add 0 ℃ ~ 5 ℃ the frozen water of 1000ml; Under the stirring of electric mixer, be added dropwise to 10ml hydrochloric acid and 20ml titanium tetrachloride, generate the titanium tetrachloride hydrochloric acid soln; With in 10% the sodium hydroxide solution with the titanium tetrachloride hydrochloric acid soln; Control solution temperature≤5 ℃, pH value 7.0 ~ 8.0 precipitates metatitanic acid and separates out in≤5 ℃ cold water;
B, new sedimentary metatitanic acid are removed cl ions with distilled water wash;
After the metatitanic acid of c, washing removal cl ions removes the part planar water with whizzer, promptly can be used for acid and dissolve chelating.
(2) preparation of Hydrocerol A titanium chelate:
The preparation of a, Hydrocerol A-metatitanic acid suspension mixed solution:
Titaniferous is 8.7g in the prepared metatitanic acid of the titanium tetrachloride of 20ml; In titanium: the ratio proportioning of the mol ratio 1:4 of Hydrocerol A; Add Citric acid monohydrate Food grade crystallization powder 153g at metatitanic acid; Be stirred in the planar water that solid citric acid is dissolved in metatitanic acid with electric mixer, form Hydrocerol A-metatitanic acid suspended mixture;
B, microwave hot melt chelating technology synthesizing citric acid titanium:
Hydrocerol A-metatitanic acid suspension mixed solution is placed in the special disc type teflon resin reaction vessel; With cabinet type microwave stove hot melt chelating under 100 ℃ ~ 120 ℃ temperature of 2450MHz frequency 1000W, reaction end is that milky suspension mixed solution becomes water white glue;
The preparation of c, Hydrocerol A titanium saturated solution:
Hydrocerol A titanium glue with microwave hot melt chelating is processed becomes Hydrocerol A titanium saturated solution with distilled water diluting when glue is in the hot melt state.
(3) with prepared organic titanium-the plant method of vinegar ammonium salt multifunctional organic fertilizer material of saltouing:
A, alkalescence are planted the preparation of vinegar ammonium salt compound:
To plant vinegar (containing wooden vinegar, bamboo vinegar, careless vinegar), to use volatile salt or solution of ammonium hydroxide to regulate pH be 8.0 ~ 12.0, and clarification filtration is removed materials such as tar, benzopyrene, filtrates and plant the vinegar ammonium salt compound for alkalescence;
B, acid Hydrocerol A titanium-the plant preparation of vinegar ammonium salt compound:
Hydrocerol A titanium saturated solution is regulated pH to 1.5 ~ 2.5 with the vinegar ammonium salt compound of planting of alkalescence; Make the Hydrocerol A titanium and plant the vinegar ammonium salt compound and form the gel object and separate out; Ageing is after 24 hours in≤25 ℃ of room temperatures; Remove surface adsorption water at 60 ℃ of hot blasts, be the acid Hydrocerol A titanium of leather hard-the plant composite salt of vinegar ammonium salt compound
C, organic titanium-the plant preparation of vinegar ammonium salt compound multifunctional organic fertilizer:
With leather hard the Hydrocerol A titanium-planting the vinegar ammonium salt compound mixes with the part by weight of Carbon Dioxide ammonium by 1.0:1.5, finally controlling its pH is 5.5 ~ 6.5, organic titanium-plant vinegar ammonium salt compound multifunctional organic fertilizer material is processed in oven dry in 60 ℃ ± 5 ℃ baking oven.
Embodiment 4
(1) preparation of metatitanic acid:
A, in the beaker of 1500ml, add 0 ℃ ~ 5 ℃ the frozen water of 1000ml; Under the stirring of electric mixer; Add 25g titanium sulfate stirring and dissolving, the sodium hydroxide solution neutralisation of sulphuric acid titanium solution with 10% is controlled solution temperature≤5 ℃; PH value 7.0 ~ 8.0 precipitates metatitanic acid and separates out in≤5 ℃ cold water;
B, new sedimentary metatitanic acid are removed sulfonium ion with distilled water wash;
After the metatitanic acid of c, washing removal sulfonium ion removes the part planar water with whizzer, promptly can be used for acid and dissolve chelating.
(2) preparation of Hydrocerol A titanium chelate:
The preparation of a, Hydrocerol A-metatitanic acid suspension mixed solution:
Titaniferous is 5g in the prepared metatitanic acid of 25g titanium sulfate; In titanium: the ratio proportioning of the mol ratio 1:3 of Hydrocerol A; Add Citric acid monohydrate Food grade crystallization powder 65g at metatitanic acid; Be stirred in the planar water that solid citric acid is dissolved in metatitanic acid with electric mixer, form Hydrocerol A-metatitanic acid suspended mixture;
B, microwave hot melt chelating technology synthesizing citric acid titanium:
Hydrocerol A-metatitanic acid suspension mixed solution is placed in the special disc type teflon resin reaction vessel; With cabinet type microwave stove hot melt chelating under 100 ℃ ~ 120 ℃ temperature of 2450MHz frequency 1000W, reaction end is that milky suspension mixed solution becomes water white glue;
The preparation of c, Hydrocerol A titanium saturated solution:
Hydrocerol A titanium glue with microwave hot melt chelating is processed becomes Hydrocerol A titanium saturated solution with distilled water diluting when glue is in the hot melt state.
(3) with prepared organic titanium-the plant method of vinegar ammonium salt multifunctional organic fertilizer material of saltouing:
A, alkalescence are planted the preparation of vinegar ammonium salt compound:
To plant vinegar (containing wooden vinegar, bamboo vinegar, careless vinegar), to use volatile salt or solution of ammonium hydroxide to regulate pH be 8.0 ~ 12.0, and clarification filtration is removed materials such as tar, benzopyrene, filtrates and plant the vinegar ammonium salt compound for alkalescence;
B, acid Hydrocerol A titanium-the plant preparation of vinegar ammonium salt compound:
Hydrocerol A titanium saturated solution is regulated pH to 1.5 ~ 2.5 with the vinegar ammonium salt compound of planting of alkalescence; Make the Hydrocerol A titanium and plant the vinegar ammonium salt compound and form the gel object and separate out; Ageing is after 24 hours in≤25 ℃ of room temperatures; Remove surface adsorption water at 60 ℃ of hot blasts, be the acid Hydrocerol A titanium of leather hard-the plant composite salt of vinegar ammonium salt compound
C, organic titanium-the plant preparation of vinegar ammonium salt compound multifunctional organic fertilizer:
With leather hard the Hydrocerol A titanium-planting the vinegar ammonium salt compound mixes with the part by weight of Carbon Dioxide ammonium by 1.0:1.0, finally controlling its pH is 5.5 ~ 6.5, organic titanium-plant vinegar ammonium salt compound multifunctional organic fertilizer material is processed in oven dry in 60 ℃ ± 5 ℃ baking oven.
Embodiment 5
(1) preparation of metatitanic acid:
A, in the beaker of 1500ml, add 0 ℃ ~ 5 ℃ the frozen water of 1000ml; Under the stirring of electric mixer; Add 25g titanium sulfate stirring and dissolving, the sodium hydroxide solution neutralisation of sulphuric acid titanium solution with 10% is controlled solution temperature≤5 ℃; PH value 7.0 ~ 8.0 precipitates metatitanic acid and separates out in≤5 ℃ cold water;
B, new sedimentary metatitanic acid are removed sulfonium ion with distilled water wash;
After the metatitanic acid of c, washing removal sulfonium ion removes the part planar water with whizzer, promptly can be used for acid and dissolve chelating.
(2) preparation of Hydrocerol A titanium chelate:
The preparation of a, Hydrocerol A-metatitanic acid suspension mixed solution:
Titaniferous is 5g in the prepared metatitanic acid of 25g titanium sulfate; In titanium: the ratio proportioning of the mol ratio 1:2.5 of Hydrocerol A; Add Citric acid monohydrate Food grade crystallization powder 54g at metatitanic acid; Be stirred in the planar water that solid citric acid is dissolved in metatitanic acid with electric mixer, form Hydrocerol A-metatitanic acid suspended mixture;
B, microwave hot melt chelating technology synthesizing citric acid titanium:
Hydrocerol A-metatitanic acid suspension mixed solution is placed in the special disc type teflon resin reaction vessel; With cabinet type microwave stove hot melt chelating under 100 ℃ ~ 120 ℃ temperature of 2450MHz frequency 1000W, reaction end is that milky suspension mixed solution becomes water white glue;
The preparation of c, Hydrocerol A titanium saturated solution:
Hydrocerol A titanium glue with microwave hot melt chelating is processed becomes Hydrocerol A titanium saturated solution with distilled water diluting when glue is in the hot melt state.
(3) with prepared organic titanium-the plant method of vinegar ammonium salt multifunctional organic fertilizer material of saltouing:
A, alkalescence are planted the preparation of vinegar ammonium salt compound:
To plant vinegar (containing wooden vinegar, bamboo vinegar, careless vinegar), to use volatile salt or solution of ammonium hydroxide to regulate pH be 8.0 ~ 12.0, and clarification filtration is removed materials such as tar, benzopyrene, filtrates and plant the vinegar ammonium salt compound for alkalescence;
B, acid Hydrocerol A titanium-the plant preparation of vinegar ammonium salt compound:
Hydrocerol A titanium saturated solution is regulated pH to 1.5 ~ 2.5 with the vinegar ammonium salt compound of planting of alkalescence; Make the Hydrocerol A titanium and plant the vinegar ammonium salt compound and form the gel object and separate out; Ageing is after 24 hours in≤25 ℃ of room temperatures; Remove surface adsorption water at 60 ℃ of hot blasts, be the acid Hydrocerol A titanium of leather hard-the plant composite salt of vinegar ammonium salt compound
C, organic titanium-the plant preparation of vinegar ammonium salt compound multifunctional organic fertilizer:
With leather hard the Hydrocerol A titanium-planting the vinegar ammonium salt compound mixes with the part by weight of Carbon Dioxide ammonium by 1.0:0.8, finally controlling its pH is 5.5 ~ 6.5, organic titanium-plant vinegar ammonium salt compound multifunctional organic fertilizer material is processed in oven dry in 60 ℃ ± 5 ℃ baking oven.
Embodiment 6
(1) preparation of metatitanic acid:
A, in the beaker of 1500ml, add 0 ℃ ~ 5 ℃ the frozen water of 1000ml; Under the stirring of electric mixer; Add 25g titanium sulfate stirring and dissolving, the sodium hydroxide solution neutralisation of sulphuric acid titanium solution with 10% is controlled solution temperature≤5 ℃; PH value 7.0 ~ 8.0 precipitates metatitanic acid and separates out in≤5 ℃ cold water;
B, new sedimentary metatitanic acid are removed sulfonium ion with distilled water wash;
After the metatitanic acid of c, washing removal sulfonium ion removes the part planar water with whizzer, promptly can be used for acid and dissolve chelating.
(2) preparation of Hydrocerol A titanium chelate:
The preparation of a, Hydrocerol A-metatitanic acid suspension mixed solution:
Titaniferous is 5g in the prepared metatitanic acid of 25g titanium sulfate; In titanium: the ratio proportioning of the mol ratio 1:3 of Hydrocerol A; Add Citric acid monohydrate Food grade crystallization powder 86g at metatitanic acid; Be stirred in the planar water that solid citric acid is dissolved in metatitanic acid with electric mixer, form Hydrocerol A-metatitanic acid suspended mixture;
B, microwave hot melt chelating technology synthesizing citric acid titanium:
Hydrocerol A-metatitanic acid suspension mixed solution is placed in the special disc type teflon resin reaction vessel; With cabinet type microwave stove hot melt chelating under 100 ℃ ~ 120 ℃ temperature of 2450MHz frequency 1000W, reaction end is that milky suspension mixed solution becomes water white glue;
The preparation of c, Hydrocerol A titanium saturated solution:
Hydrocerol A titanium glue with microwave hot melt chelating is processed becomes Hydrocerol A titanium saturated solution with distilled water diluting when glue is in the hot melt state.
(3) with prepared organic titanium-the plant method of vinegar ammonium salt multifunctional organic fertilizer material of saltouing:
A, alkalescence are planted the preparation of vinegar ammonium salt compound:
To plant vinegar (containing wooden vinegar, bamboo vinegar, careless vinegar), to use volatile salt or solution of ammonium hydroxide to regulate pH be 8.0 ~ 12.0, and clarification filtration is removed materials such as tar, benzopyrene, filtrates and plant the vinegar ammonium salt compound for alkalescence;
B, acid Hydrocerol A titanium-the plant preparation of vinegar ammonium salt compound:
Hydrocerol A titanium saturated solution is regulated pH to 1.5 ~ 2.5 with the vinegar ammonium salt compound of planting of alkalescence; Make the Hydrocerol A titanium and plant the vinegar ammonium salt compound and form the gel object and separate out; Ageing is after 24 hours in≤25 ℃ of room temperatures; Remove surface adsorption water at 60 ℃ of hot blasts, be the acid Hydrocerol A titanium of leather hard-the plant composite salt of vinegar ammonium salt compound
C, organic titanium-the plant preparation of vinegar ammonium salt compound multifunctional organic fertilizer:
With leather hard the Hydrocerol A titanium-planting the vinegar ammonium salt compound mixes with the part by weight of Carbon Dioxide ammonium by 1.0:1.5, finally controlling its pH is 5.5 ~ 6.5, organic titanium-plant vinegar ammonium salt compound multifunctional organic fertilizer material is processed in oven dry in 60 ℃ ± 5 ℃ baking oven.
More than be embodiment of the present invention, all similar changes of doing according to above-mentioned design ought to belong to the content that contains of the present invention.
Claims (5)
1. one kind with the prepared organic titanium of saltouing-plant the method for vinegar ammonium salt fertilizer, it is characterized in that:
A, with in the alkali and a kind of not chloride, sulfonium ion of the frozen water formulations prepared from solutions of titanium salt, can be dissolved in the new deposition metatitanic acid of Hydrocerol A,
B, with not chloride, sulfonium ion, can be dissolved in the new deposition metatitanic acid of Hydrocerol A, the muriate of instead of titanium, vitriol be as the raw material of the Hydrocerol A titanium of synthetic not chloride, sulfonium ion,
C, not chloride, the sulfonium ion of usefulness, the new deposition metatitanic acid that can be dissolved in Hydrocerol A is the titanium source, is sour solvent, sequestrant with Hydrocerol A, synthesizes Hydrocerol A titanium not chloride, sulfonium ion with microwave hot melt chelating technology,
D, Hydrocerol A titanium saturated solution is planted vinegar ammonium salt compound neutralization preparation organic titanium-the plant vinegar ammonium salt compound multifunctional organic fertilizer material of saltouing with alkalescence.
2. saltout prepared organic titanium-plant the method for vinegar ammonium salt fertilizer of a kind of usefulness according to claim 1, it is characterized in that described with in the alkali with the frozen water solution of titanium salt, the new deposition metatitanic acid of preparation, preparation according to the following steps:
A, the vitriol of the muriate of titanium or titanium is dissolved among the frozen water, with the neutralization of 10% ~ 30% sodium hydroxide solution, control pH is 7.0 ~ 8.0, and deposition is separated out oyster white gel metatitanic acid in≤5 ℃ cold water,
B, new sedimentary metatitanic acid are removed cl ions or sulfonium ion with distilled water wash,
After the new sedimentary metatitanic acid of c, washing removal cl ions or sulfonium ion removes the part planar water with whizzer, in time be used for acid and dissolve chelating.
3. saltout prepared organic titanium-plant the method for vinegar ammonium salt fertilizer of a kind of usefulness according to claim 1 is characterized in that described new deposition metatitanic acid and the Hydrocerol A ratio proportioning in titanium: Hydrocerol A=1:2.5 ~ 4 mol ratios.
4. saltout prepared organic titanium-plant the method for vinegar ammonium salt fertilizer of a kind of usefulness according to claim 1, it is characterized in that described with microwave hot melt chelating technology according to the following steps:
The preparation of a, Hydrocerol A-metatitanic acid suspension mixed solution:
In titanium: the ratio proportioning of the mol ratio 1:2.5 of Hydrocerol A ~ 4, the Citric acid monohydrate Food grade of xln is dissolved in the planar water of new deposition metatitanic acid, stirring generates milky Hydrocerol A-metatitanic acid suspension mixed solution,
B, microwave hot melt chelating technology synthesizing citric acid titanium:
Hydrocerol A-metatitanic acid suspension mixed solution is placed in the special disc type teflon resin reaction vessel; With operating frequency 915MHz or use operating frequency 2450MHz; The cabinet type microwave device of microwave power 1 ~ 10KW, or tunnel type micro wave equipment carries out radiation hot melt chelating, and the microwave thermal melting temperatur is controlled at 100 ℃ ~ 120 ℃; Reaction end is that milky suspension mixed solution becomes water white glue
The preparation of c, Hydrocerol A titanium saturated solution:
Hydrocerol A titanium glue with microwave hot melt chelating is processed when glue also is in the hot melt state, becomes Hydrocerol A titanium saturated solution with distilled water diluting.
5. saltout prepared organic titanium-plant the method for vinegar ammonium salt fertilizer of a kind of usefulness according to claim 1 is characterized in that described Hydrocerol A titanium saturated solution saltouts technology according to the following steps with the vinegar ammonium salt compound neutralization of planting of alkalescence:
A, alkalescence are planted the preparation of vinegar ammonium salt compound,
To plant vinegar (containing wooden vinegar, bamboo vinegar, careless vinegar), to use volatile salt or solution of ammonium hydroxide to regulate pH be 8.0 ~ 9.0, and clarification filtration is removed materials such as tar, benzopyrene, filtrate and plant the vinegar ammonium salt compound for alkalescence,
B, acid Hydrocerol A titanium-the plant preparation of vinegar ammonium salt compound:
Hydrocerol A titanium saturated solution is regulated pH to 1.5 ~ 2.5 with the vinegar ammonium salt compound of planting of alkalescence; Make the Hydrocerol A titanium and plant the vinegar ammonium salt compound and form the gel object and separate out; Ageing is after 24 hours in≤25 ℃ of room temperatures; Remove surface adsorption water at 60 ℃ of hot blasts, be the acid Hydrocerol A titanium of leather hard-the plant composite salt of vinegar ammonium salt compound
C, organic titanium-the plant preparation of vinegar ammonium salt compound multifunctional organic fertilizer:
With the Hydrocerol A titanium of leather hard-plant vinegar ammonium salt compound and Carbon Dioxide ammonium proportional mixing, finally controlling its pH is 5.5 ~ 6.0, and organic titanium-plant vinegar ammonium salt organic fertilizer is processed in oven dry in 60 ℃ ± 5 ℃ baking oven.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107449744A (en) * | 2017-07-14 | 2017-12-08 | 纤化（上海）生物化工股份有限公司 | The analysis method of activity of catalase in a kind of detection textile printing and dyeing industry |
| CN109612870A (en) * | 2018-01-25 | 2019-04-12 | 浙江农林大学 | A kind of convenient method for measuring plant vinegar liquid total organic matter and moisture content |
| CN110615711A (en) * | 2019-09-25 | 2019-12-27 | 正大农业科技(浙江)有限公司 | Soil conditioner for adjusting salinity and alkalinity and preparation method thereof |
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| JPS544760A (en) * | 1977-06-13 | 1979-01-13 | Daiken Kakou Kk | Production of silicic acid composite fertilizer |
| CN1052302A (en) * | 1989-11-28 | 1991-06-19 | 北京有色金属研究总院 | Titanium compound for plant growing regulating agent and synthetic |
| KR20010079321A (en) * | 2001-07-06 | 2001-08-22 | 오근호 | Microwave omitted |
| KR20050052043A (en) * | 2003-11-28 | 2005-06-02 | 박만조 | The recipe of life-activating fertilizer for environment-friendly farming |
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2011
- 2011-12-13 CN CN201110412121.3A patent/CN102531772B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS544760A (en) * | 1977-06-13 | 1979-01-13 | Daiken Kakou Kk | Production of silicic acid composite fertilizer |
| CN1052302A (en) * | 1989-11-28 | 1991-06-19 | 北京有色金属研究总院 | Titanium compound for plant growing regulating agent and synthetic |
| KR20010079321A (en) * | 2001-07-06 | 2001-08-22 | 오근호 | Microwave omitted |
| KR20050052043A (en) * | 2003-11-28 | 2005-06-02 | 박만조 | The recipe of life-activating fertilizer for environment-friendly farming |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107449744A (en) * | 2017-07-14 | 2017-12-08 | 纤化（上海）生物化工股份有限公司 | The analysis method of activity of catalase in a kind of detection textile printing and dyeing industry |
| CN109612870A (en) * | 2018-01-25 | 2019-04-12 | 浙江农林大学 | A kind of convenient method for measuring plant vinegar liquid total organic matter and moisture content |
| CN110615711A (en) * | 2019-09-25 | 2019-12-27 | 正大农业科技(浙江)有限公司 | Soil conditioner for adjusting salinity and alkalinity and preparation method thereof |
| CN110615711B (en) * | 2019-09-25 | 2021-09-17 | 正大农业科技(浙江)有限公司 | Soil conditioner for adjusting salinity and alkalinity and preparation method thereof |
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| CN102531772B (en) | 2014-06-18 |
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