CN111138212A - Preparation method of compound fertilizer with biological slow release function - Google Patents

Preparation method of compound fertilizer with biological slow release function Download PDF

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Publication number
CN111138212A
CN111138212A CN201911374242.6A CN201911374242A CN111138212A CN 111138212 A CN111138212 A CN 111138212A CN 201911374242 A CN201911374242 A CN 201911374242A CN 111138212 A CN111138212 A CN 111138212A
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Prior art keywords
urea
formaldehyde
reaction
user
slow release
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吴安昌
张卫卫
华古文
周传胜
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Anhui Huilong Group Wuhe Ecological Fertilizer Industry Co ltd
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Anhui Huilong Group Wuhe Ecological Fertilizer Industry Co ltd
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Priority to CN201911374242.6A priority Critical patent/CN111138212A/en
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    • C—CHEMISTRY; METALLURGY
    • C05—FERTILISERS; MANUFACTURE THEREOF
    • C05C—NITROGENOUS FERTILISERS
    • C05C9/00—Fertilisers containing urea or urea compounds
    • C05C9/02—Fertilisers containing urea or urea compounds containing urea-formaldehyde condensates
    • C—CHEMISTRY; METALLURGY
    • C05—FERTILISERS; MANUFACTURE THEREOF
    • C05B—PHOSPHATIC FERTILISERS
    • C05B7/00—Fertilisers based essentially on alkali or ammonium orthophosphates
    • C—CHEMISTRY; METALLURGY
    • C05—FERTILISERS; MANUFACTURE THEREOF
    • C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
    • C05G1/00—Mixtures of fertilisers belonging individually to different subclasses of C05
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C273/00—Preparation of urea or its derivatives, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups
    • C07C273/18—Preparation of urea or its derivatives, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups of substituted ureas
    • C07C273/1854—Preparation of urea or its derivatives, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups of substituted ureas by reactions not involving the formation of the N-C(O)-N- moiety
    • C07C273/1863—Preparation of urea or its derivatives, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups of substituted ureas by reactions not involving the formation of the N-C(O)-N- moiety from urea
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P60/00—Technologies relating to agriculture, livestock or agroalimentary industries
    • Y02P60/20—Reduction of greenhouse gas [GHG] emissions in agriculture, e.g. CO2
    • Y02P60/21—Dinitrogen oxide [N2O], e.g. using aquaponics, hydroponics or efficiency measures

Abstract

The invention provides a preparation method of a compound fertilizer with a biological slow release function, which comprises the following steps of preparing raw materials of urea, formaldehyde (Io (HCHO) 38% aqueous solution), sodium hydroxide, phosphoric acid, potash fertilizer and organic fertilizer; the preparation instrument is as follows: a 600mL three-neck flask, an electric stirrer, a constant temperature water bath, a thermometer, an analytical balance, a nitrogen determination instrument, a Buchner funnel, a filter flask, a rubber tube, an air pump and filter paper. The invention can improve the chemical reaction rate and effect of the urea-formaldehyde reactant by matching the processes of the step A, the step B, the step C, the step D and the step E, further purify, filter and purify the urea-formaldehyde reactant by suction filtration, reduce impurities in the urea-formaldehyde reactant, dry the urea-formaldehyde reactant into a solid form by drying, and then obtain a high-efficiency long-acting urea-formaldehyde compound fertilizer solid particle finished product integrating slow release and controlled release into a whole by a granulation finished product process, wherein the conversion rate of nitrogen is higher than 40%.

Description

Preparation method of compound fertilizer with biological slow release function
Technical Field
The invention relates to the field of compound fertilizers, in particular to a preparation method of a compound fertilizer with a biological slow release function.
Background
The compound fertilizer is a chemical fertilizer containing any two or three of crop nutrient elements of nitrogen, phosphorus and potassium, and is prepared by a chemical method or a mixing method, the urea-formaldehyde compound fertilizer is a colloid of 1 methylene-2 urea and 2 methylene urea which are generated by the reaction of urea and formaldehyde at high temperature, and is mainly used on the lawn of a golf course and is also the only compound fertilizer which can be used for drip irrigation at present.
All need use compound fertilizer when the grower carries out lawn fertilization management to organic crop or golf course, however current compound fertilizer preparation method does not possess biological slow-release function, mostly belongs to low end fertilizer, and the conversion rate of nitrogen is mostly less than 40%, and the harmful substance of leaving over in the soil simultaneously is more, causes the pollution to the soil environment and the water source of fertilizeing, also can not provide better nutritive environment to the plant simultaneously.
Therefore, there is a need to provide a method for preparing a compound fertilizer with biological slow release function to solve the above technical problems.
Disclosure of Invention
The invention provides a preparation method of a compound fertilizer with a biological slow release function, which solves the problem that the existing preparation method of the compound fertilizer does not have the biological slow release function.
In order to solve the technical problems, the invention provides a preparation method of a compound fertilizer with a biological slow release function, which comprises the following steps of preparing raw materials of urea, formaldehyde (Io (HCHO) 38% aqueous solution), sodium hydroxide, phosphoric acid, potash fertilizer and organic fertilizer;
the preparation instrument is as follows: a 600mL three-neck flask, an electric stirrer, a constant-temperature water bath, a thermometer, an analytical balance, a nitrogen determination instrument, a Buchner funnel, a filter flask, a rubber tube, an air pump and filter paper;
the preparation method comprises the following steps:
A. stirring: a user respectively adds 108.8g of urea and 210.6mL of water into a 600mL three-neck flask, places the mixture into a constant-temperature water bath kettle, and starts an electric stirrer to uniformly stir and mix the raw materials added into the 600mL three-neck flask for 1-2 h;
B. acid-base reaction: adding a certain amount of NaOH solution to adjust the pH value to be alkalescent, adding 120g of formaldehyde solution, adding a certain amount of HPO into a user, and adjusting the pH value of the solution to be acidic;
C. and (3) suction filtration: a user connects the buchner funnel with the suction flask in advance, then connects the air pump with the suction flask tightly through the rubber tube, and then the air pump carries out vacuum filtration treatment on the obtained reactant on the filter paper;
D. drying: drying the reaction product after suction filtration in a drying oven at 90 ℃ for 2h, determining the activity index of the product by a user according to a standard established by AOAC, and analyzing an experimental result to obtain a prepared urea-formaldehyde reaction product;
e: and (4) granulating to obtain a finished product: according to the situation of on-site demand, geometric multiple increase is carried out on the proportion of the raw materials, and then a user places the urea-formaldehyde reactant, a certain amount of monoammonium phosphate, the potash fertilizer and the organic fertilizer into a disc granulator for large-scale granulation production, so as to obtain a high-efficiency long-acting urea-formaldehyde compound fertilizer solid particle finished product integrating slow release and controlled release;
the urea formaldehyde is prepared by the following two steps of reaction of formaldehyde and urea, and the chemical formula is as follows:
a. hydroxymethylation reaction under alkaline conditions, formaldehyde and urea react to form methylol urea:
HCHO+H2NCONH2→H2NCONHCH2OH (1)
HCH0+H2NCONHCH2OH→HOCH2NHCONHCH2OH(2)
b. the methylene reaction is carried out under the acidic condition, the hydroxymethyl urea reacts with excessive urea to generate methylene diurea and dimethylene triurea, the methylene diurea and dimethylene triurea continuously react with the hydroxymethyl urea to generate the poly methylene urea with higher polymerization degree,
H2NCONHCH2OH+H2NCO1NH2→H2NCONHCH2NHCO2NH2+H2O (3)
HOCH2NHCONHCH2OH+2H2NCONH2→H2NCOHNCH2NHCONHCH2NHCONH2+2H2O (4)
the polymethylene urea has the general formula: h2NCONH(CH2NHCONH)nH, wherein n is 1-10.
Preferably, the model of the azotometer is KDN-08A, a certain amount of NaOH needs to be added when the temperature of the thermostatic waterbath is raised to 50 ℃ during the alkaline reaction in the step B, the reaction time is 2 hours, HPO is added during the acidic reaction in the step B, the temperature is kept unchanged at 50 ℃, and the reaction is terminated after the reaction is carried out for 2 hours.
Preferably, in the step D, the user dries the urea-formaldehyde compound fertilizer for 2 hours at four temperature conditions of 80 ℃, 90 ℃, 100 ℃ and 110 ℃, the activity index of the product is measured, the drying temperature of the product is obtained through comparison, and then the urea-formaldehyde compound fertilizer with the best slow release effect is prepared.
Preferably, the temperature during the hydroxymethylation reaction is controlled to be 45-80 ℃, and in order to reduce energy consumption, the temperature is selected to be 45 ℃ by a user, and the reaction time is 2.5 h.
Preferably, the temperature during the b-methylenation reaction is maintained between 35 ℃ and 60 ℃, and the temperature selected by the user is 40 ℃ and the reaction time is 2 h.
Preferably, the step a is carried out under alkaline conditions during the hydroxymethylation reaction, the pH value of the alkaline solution is 7-10, NaOH, K0H and Na2CO3All can be used for the pH value of the hydroxymethylation reaction, and NaOH is selected by a user.
Preferably, the process of the b-methylenation reaction is carried out under acidic conditions, the pH value of the acidic solution is controlled to be 3-5, and the user can select phosphoric acid, sulfuric acid, hydrochloric acid and the like for adjustment, and the phosphoric acid can provide phosphorus necessary for crops, so the user selects phosphoric acid as the acidic solution.
Compared with the related technology, the preparation method of the compound fertilizer with the biological slow release function provided by the invention has the following beneficial effects:
the invention provides a preparation method of a compound fertilizer with a biological slow release function,
1. the invention can improve the chemical reaction rate and effect of the urea-formaldehyde reactant by matching the flows of the steps A, B, C, D and E, further purify, filter and purify the urea-formaldehyde reactant by suction filtration, reduce impurities in the urea-formaldehyde reactant, dry the urea-formaldehyde reactant into a solid form by drying, and then obtain a urea-formaldehyde compound fertilizer solid particle finished product which has high efficiency, long acting and integrates slow release and controlled release into a whole by a granulation finished product process, wherein the nitrogen conversion rate is higher than 40%, and harmful substances left in soil are reduced, so that the pollution of the compound fertilizer to the soil environment and peripheral water sources is prevented;
2. according to the invention, raw materials such as urea and water are mixed and stirred through the stirring in the step A, raw material support is provided for the next process, the raw materials are subjected to acid-base chemical reaction through the acid-base reaction in the step B to obtain fertilizer crystals, the fertilizer crystals are subjected to suction filtration in the step C and drying in the step D, then the obtained fertilizer crystals are subjected to further impurity filtration to ensure the purity of the fertilizer, and the purified fertilizer crystals can be granulated to obtain finished products through the step E.
Drawings
FIG. 1 is a diagram of the synthesis reaction conditions of a preferred embodiment of the method for preparing a compound fertilizer with biological slow release function according to the present invention.
Detailed Description
The invention is further described with reference to the following figures and embodiments.
Referring to fig. 1, fig. 1 is a synthesis reaction condition diagram of a preferred embodiment of a method for preparing a compound fertilizer with a biological slow-release function according to the present invention, wherein the raw materials of the method for preparing a compound fertilizer with a biological slow-release function include urea, formaldehyde (io (hcho) 38% aqueous solution), sodium hydroxide, phosphoric acid, potash fertilizer, and organic fertilizer;
the preparation instrument is as follows: a 600mL three-neck flask, an electric stirrer, a constant-temperature water bath, a thermometer, an analytical balance, a nitrogen determination instrument, a Buchner funnel, a filter flask, a rubber tube, an air pump and filter paper;
the preparation method comprises the following steps:
A. stirring: a user respectively adds 108.8g of urea and 210.6mL of water into a 600mL three-neck flask, places the mixture into a constant-temperature water bath kettle, and starts an electric stirrer to uniformly stir and mix the raw materials added into the 600mL three-neck flask for 1-2 h;
B. acid-base reaction: adding a certain amount of NaOH solution to adjust the pH value to be alkalescent, adding 120g of formaldehyde solution, adding a certain amount of HPO into a user, and adjusting the pH value of the solution to be acidic;
C. and (3) suction filtration: a user connects the buchner funnel with the suction flask in advance, then connects the air pump with the suction flask tightly through the rubber tube, and then the air pump carries out vacuum filtration treatment on the obtained reactant on the filter paper;
D. drying: drying the reaction product after suction filtration in a drying oven at 90 ℃ for 2h, determining the activity index of the product by a user according to a standard established by AOAC, and analyzing an experimental result to obtain a prepared urea-formaldehyde reaction product;
e: and (4) granulating to obtain a finished product: according to the situation of on-site demand, geometric multiple increase is carried out on the proportion of the raw materials, and then a user places the urea-formaldehyde reactant, a certain amount of monoammonium phosphate, the potash fertilizer and the organic fertilizer into a disc granulator for large-scale granulation production, so as to obtain a high-efficiency long-acting urea-formaldehyde compound fertilizer solid particle finished product integrating slow release and controlled release;
the urea formaldehyde is prepared by the following two steps of reaction of formaldehyde and urea, and the chemical formula is as follows:
a. hydroxymethylation reaction under alkaline conditions, formaldehyde and urea react to form methylol urea:
HCHO+H2NCONH2→H2NCONHCH2OH (1)
HCH0+H2NCONHCH2OH→HOCH2NHCONHCH2OH (2)
b. the methylene reaction is carried out under the acidic condition, the hydroxymethyl urea reacts with excessive urea to generate methylene diurea and dimethylene triurea, the methylene diurea and dimethylene triurea continuously react with the hydroxymethyl urea to generate the poly methylene urea with higher polymerization degree,
H2NCONHCH2OH+H2NCO1NH2→H2NCONHCH2NHCO2NH2+H2O (3)
HOCH2NHCONHCH2OH+2H2NCONH2→H2NCOHNCH2NHCONHCH2NHCONH2+2H2O (4)
the polymethylene urea has the general formula: h2NCONH(CH2NHCONH)nH, wherein n is 1-10.
The first embodiment is as follows:
a method for preparing compound fertilizer with biological slow release function comprises preparing raw materials of urea, formaldehyde (Io (HCHO) 38% aqueous solution), sodium hydroxide, phosphoric acid, potash fertilizer and organic fertilizer;
the preparation instrument is as follows: a 600mL three-neck flask, an electric stirrer, a constant-temperature water bath, a thermometer, an analytical balance, a nitrogen determination instrument, a Buchner funnel, a filter flask, a rubber tube, an air pump and filter paper;
the preparation method comprises the following steps:
A. stirring: a user respectively adds 108.8g of urea and 210.6mL of water into a 600mL three-neck flask, places the mixture into a constant-temperature water bath kettle, and starts an electric stirrer to uniformly stir and mix the raw materials added into the 600mL three-neck flask for 1-2 h;
B. acid-base reaction: adding a certain amount of NaOH solution to adjust the pH value to be alkalescent, adding 120g of formaldehyde solution, adding a certain amount of HPO into a user, and adjusting the pH value of the solution to be acidic;
C. and (3) suction filtration: a user connects the buchner funnel with the suction flask in advance, then connects the air pump with the suction flask tightly through the rubber tube, and then the air pump carries out vacuum filtration treatment on the obtained reactant on the filter paper;
D. drying: drying the reaction product after suction filtration in a drying oven at 90 ℃ for 2h, determining the activity index of the product by a user according to a standard established by AOAC, and analyzing an experimental result to obtain a prepared urea-formaldehyde reaction product;
e: and (4) granulating to obtain a finished product: according to the situation of on-site demand, geometric multiple increase is carried out on the proportion of the raw materials, and then a user places the urea-formaldehyde reactant, a certain amount of monoammonium phosphate, the potash fertilizer and the organic fertilizer into a disc granulator for large-scale granulation production, so as to obtain a high-efficiency long-acting urea-formaldehyde compound fertilizer solid particle finished product integrating slow release and controlled release;
the urea formaldehyde is prepared by the following two steps of reaction of formaldehyde and urea, and the chemical formula is as follows:
a. hydroxymethylation reaction under alkaline conditions, formaldehyde and urea react to form methylol urea:
HCHO+H2NCONH2→H2NCONHCH2OH (1)
HCH0+H2NCONHCH2OH→HOCH2NHCONHCH2OH (2)
b. the methylene reaction is carried out under the acidic condition, the hydroxymethyl urea reacts with excessive urea to generate methylene diurea and dimethylene triurea, the methylene diurea and dimethylene triurea continuously react with the hydroxymethyl urea to generate the poly methylene urea with higher polymerization degree,
H2NCONHCH2OH+H2NCO1NH2→H2NCONHCH2NHCO2NH2+H2O (3)
HOCH2NHCONHCH2OH+2H2NCONH2→H2NCOHNCH2NHCONHCH2NHCONH2+2H2O (4)
the polymethylene urea has the general formula: h2NCONH(CH2NHCONH)nH, wherein n is 1-10.
Example two:
in example one, the following additional steps were added:
the model of the nitrogen determination instrument is KDN-08A, a certain amount of NaOH can be added only when the temperature of the constant-temperature water bath kettle is raised to 50 ℃ during the alkaline reaction in the step B, the reaction time is 2 hours, HPO is added during the acidic reaction in the step B, the temperature is kept unchanged at 50 ℃, and the reaction is terminated after the reaction for 2 hours.
A method for preparing compound fertilizer with biological slow release function comprises preparing raw materials of urea, formaldehyde (Io (HCHO) 38% aqueous solution), sodium hydroxide, phosphoric acid, potash fertilizer and organic fertilizer;
the preparation instrument is as follows: a 600mL three-neck flask, an electric stirrer, a constant-temperature water bath, a thermometer, an analytical balance, a nitrogen determination instrument, a Buchner funnel, a filter flask, a rubber tube, an air pump and filter paper;
the preparation method comprises the following steps:
A. stirring: a user respectively adds 108.8g of urea and 210.6mL of water into a 600mL three-neck flask, places the mixture into a constant-temperature water bath kettle, and starts an electric stirrer to uniformly stir and mix the raw materials added into the 600mL three-neck flask for 1-2 h;
B. acid-base reaction: adding a certain amount of NaOH solution to adjust the pH value to be alkalescent, adding 120g of formaldehyde solution, adding a certain amount of HPO into a user, and adjusting the pH value of the solution to be acidic;
C. and (3) suction filtration: a user connects the buchner funnel with the suction flask in advance, then connects the air pump with the suction flask tightly through the rubber tube, and then the air pump carries out vacuum filtration treatment on the obtained reactant on the filter paper;
D. drying: drying the reaction product after suction filtration in a drying oven at 90 ℃ for 2h, determining the activity index of the product by a user according to a standard established by AOAC, and analyzing an experimental result to obtain a prepared urea-formaldehyde reaction product;
e: and (4) granulating to obtain a finished product: according to the situation of on-site demand, geometric multiple increase is carried out on the proportion of the raw materials, and then a user places the urea-formaldehyde reactant, a certain amount of monoammonium phosphate, the potash fertilizer and the organic fertilizer into a disc granulator for large-scale granulation production, so as to obtain a high-efficiency long-acting urea-formaldehyde compound fertilizer solid particle finished product integrating slow release and controlled release;
the urea formaldehyde is prepared by the following two steps of reaction of formaldehyde and urea, and the chemical formula is as follows:
a. hydroxymethylation reaction under alkaline conditions, formaldehyde and urea react to form methylol urea:
HCHO+H2NCONH2→H2NCONHCH2OH (1)
HCH0+H2NCONHCH2OH→HOCH2NHCONHCH2OH (2)
b. the methylene reaction is carried out under the acidic condition, the hydroxymethyl urea reacts with excessive urea to generate methylene diurea and dimethylene triurea, the methylene diurea and dimethylene triurea continuously react with the hydroxymethyl urea to generate the poly methylene urea with higher polymerization degree,
H2NCONHCH2OH+H2NCO1NH2→H2NCONHCH2NHCO2NH2+H2O (3)
HOCH2NHCONHCH2OH+2H2NCONH2→H2NCOHNCH2NHCONHCH2NHCONH2+2H2O (4)
the polymethylene urea has the general formula: h2NCONH(CH2NHCONH)nH, wherein n is 1-10.
Example three:
in example two, the following additional steps were added:
and D, drying the urea-formaldehyde compound fertilizer for 2 hours at four temperature conditions of 80 ℃, 90 ℃, 100 ℃ and 110 ℃ respectively by a user, measuring the activity index of the product, and comparing to obtain the better drying temperature of the product, thereby preparing the urea-formaldehyde compound fertilizer with the optimal slow release effect.
A synthesis reaction condition diagram of a preferred embodiment, a method for preparing a compound fertilizer with a biological slow release function, which comprises the steps of preparing raw materials of urea, formaldehyde (Io (HCHO) 38% aqueous solution), sodium hydroxide, phosphoric acid, potash fertilizer and organic fertilizer;
the preparation instrument is as follows: a 600mL three-neck flask, an electric stirrer, a constant-temperature water bath, a thermometer, an analytical balance, a nitrogen determination instrument, a Buchner funnel, a filter flask, a rubber tube, an air pump and filter paper;
the preparation method comprises the following steps:
A. stirring: a user respectively adds 108.8g of urea and 210.6mL of water into a 600mL three-neck flask, places the mixture into a constant-temperature water bath kettle, and starts an electric stirrer to uniformly stir and mix the raw materials added into the 600mL three-neck flask for 1-2 h;
B. acid-base reaction: adding a certain amount of NaOH solution to adjust the pH value to be alkalescent, adding 120g of formaldehyde solution, adding a certain amount of HPO into a user, and adjusting the pH value of the solution to be acidic;
C. and (3) suction filtration: a user connects the buchner funnel with the suction flask in advance, then connects the air pump with the suction flask tightly through the rubber tube, and then the air pump carries out vacuum filtration treatment on the obtained reactant on the filter paper;
D. drying: drying the reaction product after suction filtration in a drying oven at 90 ℃ for 2h, determining the activity index of the product by a user according to a standard established by AOAC, and analyzing an experimental result to obtain a prepared urea-formaldehyde reaction product;
e: and (4) granulating to obtain a finished product: according to the situation of on-site demand, geometric multiple increase is carried out on the proportion of the raw materials, and then a user places the urea-formaldehyde reactant, a certain amount of monoammonium phosphate, the potash fertilizer and the organic fertilizer into a disc granulator for large-scale granulation production, so as to obtain a high-efficiency long-acting urea-formaldehyde compound fertilizer solid particle finished product integrating slow release and controlled release;
the urea formaldehyde is prepared by the following two steps of reaction of formaldehyde and urea, and the chemical formula is as follows:
a. hydroxymethylation reaction under alkaline conditions, formaldehyde and urea react to form methylol urea:
HCHO+H2NCONH2→H2NCONHCH2OH (1)
HCH0+H2NCONHCH2OH→HOCH2NHCONHCH2OH (2)
b. the methylene reaction is carried out under the acidic condition, the hydroxymethyl urea reacts with excessive urea to generate methylene diurea and dimethylene triurea, the methylene diurea and dimethylene triurea continuously react with the hydroxymethyl urea to generate the poly methylene urea with higher polymerization degree,
H2NCONHCH2OH+H2NCO1NH2→H2NCONHCH2NHCO2NH2+H2O (3)
HOCH2NHCONHCH2OH+2H2NCONH2→H2NCOHNCH2NHCONHCH2NHCONH2+2H2O (4)
the polymethylene urea has the general formula: h2NCONH(CH2NHCONH)nH, wherein n is 1-10
Example four:
in example three, the following additional steps were added:
the temperature is controlled to be 45-80 ℃ in the hydroxymethylation reaction process, and in order to reduce energy consumption, a user selects the temperature to be 45 ℃ and the reaction time to be 2.5 h.
A method for preparing compound fertilizer with biological slow release function comprises preparing raw materials of urea, formaldehyde (Io (HCHO) 38% aqueous solution), sodium hydroxide, phosphoric acid, potash fertilizer and organic fertilizer;
the preparation instrument is as follows: a 600mL three-neck flask, an electric stirrer, a constant-temperature water bath, a thermometer, an analytical balance, a nitrogen determination instrument, a Buchner funnel, a filter flask, a rubber tube, an air pump and filter paper;
the preparation method comprises the following steps:
A. stirring: a user respectively adds 108.8g of urea and 210.6mL of water into a 600mL three-neck flask, places the mixture into a constant-temperature water bath kettle, and starts an electric stirrer to uniformly stir and mix the raw materials added into the 600mL three-neck flask for 1-2 h;
B. acid-base reaction: adding a certain amount of NaOH solution to adjust the pH value to be alkalescent, adding 120g of formaldehyde solution, adding a certain amount of HPO into a user, and adjusting the pH value of the solution to be acidic;
C. and (3) suction filtration: a user connects the buchner funnel with the suction flask in advance, then connects the air pump with the suction flask tightly through the rubber tube, and then the air pump carries out vacuum filtration treatment on the obtained reactant on the filter paper;
D. drying: drying the reaction product after suction filtration in a drying oven at 90 ℃ for 2h, determining the activity index of the product by a user according to a standard established by AOAC, and analyzing an experimental result to obtain a prepared urea-formaldehyde reaction product;
e: and (4) granulating to obtain a finished product: according to the situation of on-site demand, geometric multiple increase is carried out on the proportion of the raw materials, and then a user places the urea-formaldehyde reactant, a certain amount of monoammonium phosphate, the potash fertilizer and the organic fertilizer into a disc granulator for large-scale granulation production, so as to obtain a high-efficiency long-acting urea-formaldehyde compound fertilizer solid particle finished product integrating slow release and controlled release;
the urea formaldehyde is prepared by the following two steps of reaction of formaldehyde and urea, and the chemical formula is as follows:
a. hydroxymethylation reaction under alkaline conditions, formaldehyde and urea react to form methylol urea:
HCHO+H2NCONH2→H2NCONHCH2OH (1)
HCH0+H2NCONHCH2OH→HOCH2NHCONHCH2OH (2)
b. the methylene reaction is carried out under the acidic condition, the hydroxymethyl urea reacts with excessive urea to generate methylene diurea and dimethylene triurea, the methylene diurea and dimethylene triurea continuously react with the hydroxymethyl urea to generate the poly methylene urea with higher polymerization degree,
H2NCONHCH2OH+H2NCO1NH2→H2NCONHCH2NHCO2NH2+H2O (3)
HOCH2NHCONHCH2OH+2H2NCONH2→H2NCOHNCH2NHCONHCH2NHCONH2+2H2O (4)
the polymethylene urea has the general formula: h2NCONH(CH2NHCONH)nH, wherein n is 1-10
Example five:
in example four, the following additional steps were added:
the temperature is maintained between 35 ℃ and 60 ℃ in the process of the b-methylenation reaction, the temperature selected by a user is 40 ℃, and the reaction time is 2 hours.
A method for preparing compound fertilizer with biological slow release function comprises preparing raw materials of urea, formaldehyde (Io (HCHO) 38% aqueous solution), sodium hydroxide, phosphoric acid, potash fertilizer and organic fertilizer;
the preparation instrument is as follows: a 600mL three-neck flask, an electric stirrer, a constant-temperature water bath, a thermometer, an analytical balance, a nitrogen determination instrument, a Buchner funnel, a filter flask, a rubber tube, an air pump and filter paper;
the preparation method comprises the following steps:
A. stirring: a user respectively adds 108.8g of urea and 210.6mL of water into a 600mL three-neck flask, places the mixture into a constant-temperature water bath kettle, and starts an electric stirrer to uniformly stir and mix the raw materials added into the 600mL three-neck flask for 1-2 h;
B. acid-base reaction: adding a certain amount of NaOH solution to adjust the pH value to be alkalescent, adding 120g of formaldehyde solution, adding a certain amount of HPO into a user, and adjusting the pH value of the solution to be acidic;
C. and (3) suction filtration: a user connects the buchner funnel with the suction flask in advance, then connects the air pump with the suction flask tightly through the rubber tube, and then the air pump carries out vacuum filtration treatment on the obtained reactant on the filter paper;
D. drying: drying the reaction product after suction filtration in a drying oven at 90 ℃ for 2h, determining the activity index of the product by a user according to a standard established by AOAC, and analyzing an experimental result to obtain a prepared urea-formaldehyde reaction product;
e: and (4) granulating to obtain a finished product: according to the situation of on-site demand, geometric multiple increase is carried out on the proportion of the raw materials, and then a user places the urea-formaldehyde reactant, a certain amount of monoammonium phosphate, the potash fertilizer and the organic fertilizer into a disc granulator for large-scale granulation production, so as to obtain a high-efficiency long-acting urea-formaldehyde compound fertilizer solid particle finished product integrating slow release and controlled release;
the urea formaldehyde is prepared by the following two steps of reaction of formaldehyde and urea, and the chemical formula is as follows:
a. hydroxymethylation reaction under alkaline conditions, formaldehyde and urea react to form methylol urea:
HCHO+H2NCONH2→H2NCONHCH2OH (1)
HCH0+H2NCONHCH2OH→HOCH2NHCONHCH2OH (2)
b. the methylene reaction is carried out under the acidic condition, the hydroxymethyl urea reacts with excessive urea to generate methylene diurea and dimethylene triurea, the methylene diurea and dimethylene triurea continuously react with the hydroxymethyl urea to generate the poly methylene urea with higher polymerization degree,
H2NCONHCH2OH+H2NCO1NH2→H2NCONHCH2NHCO2NH2+H2O (3)
HOCH2NHCONHCH2OH+2H2NCONH2→H2NCOHNCH2NHCONHCH2NHCONH2+2H2O(4)
the polymethylene urea has the general formula: h2NCONH(CH2NHCONH)nH, wherein n is 1-10
Example six:
in example five, the following additional steps were added:
the step a is carried out under alkaline conditions in the hydroxymethylation process, the pH value of an alkaline solution is preferably 7-10, and NaOH, K0H and Na2CO3All can be used for the pH value of the hydroxymethylation reaction, and NaOH is selected by a user.
A method for preparing compound fertilizer with biological slow release function comprises preparing raw materials of urea, formaldehyde (Io (HCHO) 38% aqueous solution), sodium hydroxide, phosphoric acid, potash fertilizer and organic fertilizer;
the preparation instrument is as follows: a 600mL three-neck flask, an electric stirrer, a constant-temperature water bath, a thermometer, an analytical balance, a nitrogen determination instrument, a Buchner funnel, a filter flask, a rubber tube, an air pump and filter paper;
the preparation method comprises the following steps:
A. stirring: a user respectively adds 108.8g of urea and 210.6mL of water into a 600mL three-neck flask, places the mixture into a constant-temperature water bath kettle, and starts an electric stirrer to uniformly stir and mix the raw materials added into the 600mL three-neck flask for 1-2 h;
B. acid-base reaction: adding a certain amount of NaOH solution to adjust the pH value to be alkalescent, adding 120g of formaldehyde solution, adding a certain amount of HPO into a user, and adjusting the pH value of the solution to be acidic;
C. and (3) suction filtration: a user connects the buchner funnel with the suction flask in advance, then connects the air pump with the suction flask tightly through the rubber tube, and then the air pump carries out vacuum filtration treatment on the obtained reactant on the filter paper;
D. drying: drying the reaction product after suction filtration in a drying oven at 90 ℃ for 2h, determining the activity index of the product by a user according to a standard established by AOAC, and analyzing an experimental result to obtain a prepared urea-formaldehyde reaction product;
e: and (4) granulating to obtain a finished product: according to the situation of on-site demand, geometric multiple increase is carried out on the proportion of the raw materials, and then a user places the urea-formaldehyde reactant, a certain amount of monoammonium phosphate, the potash fertilizer and the organic fertilizer into a disc granulator for large-scale granulation production, so as to obtain a high-efficiency long-acting urea-formaldehyde compound fertilizer solid particle finished product integrating slow release and controlled release;
the urea formaldehyde is prepared by the following two steps of reaction of formaldehyde and urea, and the chemical formula is as follows:
a. hydroxymethylation reaction under alkaline conditions, formaldehyde and urea react to form methylol urea:
HCHO+H2NCONH2→H2NCONHCH2OH (1)
HCH0+H2NCONHCH2OH→HOCH2NHCONHCH2OH (2)
b. the methylene reaction is carried out under the acidic condition, the hydroxymethyl urea reacts with excessive urea to generate methylene diurea and dimethylene triurea, the methylene diurea and dimethylene triurea continuously react with the hydroxymethyl urea to generate the poly methylene urea with higher polymerization degree,
H2NCONHCH2OH+H2NCO1NH2→H2NCONHCH2NHCO2NH2+H2O (3)
HOCH2NHCONHCH2OH+2H2NCONH2→H2NCOHNCH2NHCONHCH2NHCONH2+2H2O (4)
the polymethylene urea has the general formula: h2NCONH(CH2NHCONH)nH, wherein n is 1-10.
Example seven:
in example six, the following additional steps were added:
the process of the b-methylenation reaction is carried out under acidic condition, the pH value of the acidic solution is preferably controlled to be 3-5, and the user can select phosphoric acid, sulfuric acid, hydrochloric acid and the like for adjustment, and the phosphoric acid can provide phosphorus necessary for crops, so the user selects the phosphoric acid as the acidic solution.
A method for preparing compound fertilizer with biological slow release function comprises preparing raw materials of urea, formaldehyde (Io (HCHO) 38% aqueous solution), sodium hydroxide, phosphoric acid, potash fertilizer and organic fertilizer;
the preparation instrument is as follows: a 600mL three-neck flask, an electric stirrer, a constant-temperature water bath, a thermometer, an analytical balance, a nitrogen determination instrument, a Buchner funnel, a filter flask, a rubber tube, an air pump and filter paper;
the preparation method comprises the following steps:
A. stirring: a user respectively adds 108.8g of urea and 210.6mL of water into a 600mL three-neck flask, places the mixture into a constant-temperature water bath kettle, and starts an electric stirrer to uniformly stir and mix the raw materials added into the 600mL three-neck flask for 1-2 h;
B. acid-base reaction: adding a certain amount of NaOH solution to adjust the pH value to be alkalescent, adding 120g of formaldehyde solution, adding a certain amount of HPO into a user, and adjusting the pH value of the solution to be acidic;
C. and (3) suction filtration: a user connects the buchner funnel with the suction flask in advance, then connects the air pump with the suction flask tightly through the rubber tube, and then the air pump carries out vacuum filtration treatment on the obtained reactant on the filter paper;
D. drying: drying the reaction product after suction filtration in a drying oven at 90 ℃ for 2h, determining the activity index of the product by a user according to a standard established by AOAC, and analyzing an experimental result to obtain a prepared urea-formaldehyde reaction product;
e: and (4) granulating to obtain a finished product: according to the situation of on-site demand, geometric multiple increase is carried out on the proportion of the raw materials, and then a user places the urea-formaldehyde reactant, a certain amount of monoammonium phosphate, the potash fertilizer and the organic fertilizer into a disc granulator for large-scale granulation production, so as to obtain a high-efficiency long-acting urea-formaldehyde compound fertilizer solid particle finished product integrating slow release and controlled release;
the urea formaldehyde is prepared by the following two steps of reaction of formaldehyde and urea, and the chemical formula is as follows:
a. hydroxymethylation reaction under alkaline conditions, formaldehyde and urea react to form methylol urea:
HCHO+H2NCONH2→H2NCONHCH2OH (1)
HCH0+H2NCONHCH2OH→HOCH2NHCONHCH2OH (2)
b. the methylene reaction is carried out under the acidic condition, the hydroxymethyl urea reacts with excessive urea to generate methylene diurea and dimethylene triurea, the methylene diurea and dimethylene triurea continuously react with the hydroxymethyl urea to generate the poly methylene urea with higher polymerization degree,
H2NCONHCH2OH+H2NCO1NH2→H2NCONHCH2NHCO2NH2+H2O (3)
HOCH2NHCONHCH2OH+2H2NCONH2→H2NCOHNCH2NHCONHCH2NHCONH2+2H2O (4)
the polymethylene urea has the general formula: h2NCONH(CH2NHCONH)nH, wherein n is 1-10.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, which are made by using the contents of the present specification and the accompanying drawings, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.

Claims (7)

1. A method for preparing compound fertilizer with biological slow release function comprises preparing raw materials of urea, formaldehyde (Io (HCHO) 38% aqueous solution), sodium hydroxide, phosphoric acid, potash fertilizer and organic fertilizer;
the preparation instrument is as follows: a 600mL three-neck flask, an electric stirrer, a constant-temperature water bath, a thermometer, an analytical balance, a nitrogen determination instrument, a Buchner funnel, a filter flask, a rubber tube, an air pump and filter paper;
the preparation method comprises the following steps:
A. stirring: a user respectively adds 108.8g of urea and 210.6mL of water into a 600mL three-neck flask, places the mixture into a constant-temperature water bath kettle, and starts an electric stirrer to uniformly stir and mix the raw materials added into the 600mL three-neck flask for 1-2 h;
B. acid-base reaction: adding a certain amount of NaOH solution to adjust the pH value to be alkalescent, adding 120g of formaldehyde solution, adding a certain amount of HPO into a user, and adjusting the pH value of the solution to be acidic;
C. and (3) suction filtration: a user connects the buchner funnel with the suction flask in advance, then connects the air pump with the suction flask tightly through the rubber tube, and then the air pump carries out vacuum filtration treatment on the obtained reactant on the filter paper;
D. drying: drying the reaction product after suction filtration in a drying oven at 90 ℃ for 2h, determining the activity index of the product by a user according to a standard established by AOAC, and analyzing an experimental result to obtain a prepared urea-formaldehyde reaction product;
e: and (4) granulating to obtain a finished product: according to the situation of on-site demand, geometric multiple increase is carried out on the proportion of the raw materials, and then a user places the urea-formaldehyde reactant, a certain amount of monoammonium phosphate, the potash fertilizer and the organic fertilizer into a disc granulator for large-scale granulation production, so as to obtain a high-efficiency long-acting urea-formaldehyde compound fertilizer solid particle finished product integrating slow release and controlled release;
the urea formaldehyde is prepared by the following two steps of reaction of formaldehyde and urea, and the chemical formula is as follows:
a. hydroxymethylation reaction under alkaline conditions, formaldehyde and urea react to form methylol urea:
HCHO+H2NCONH2→H2NCONHCH2OH (1)
HCH0+H2NCONHCH2OH→HOCH2NHCONHCH2OH (2)
b. the methylene reaction is carried out under the acidic condition, the hydroxymethyl urea reacts with excessive urea to generate methylene diurea and dimethylene triurea, the methylene diurea and dimethylene triurea continuously react with the hydroxymethyl urea to generate the poly methylene urea with higher polymerization degree,
H2NCONHCH2OH+H2NCO1NH2→H2NCONHCH2NHCO2NH2+H2O (3)
HOCH2NHCONHCH2OH+2H2NCONH2→H2NCOHNCH2NHCONHCH2NHCONH2+2H2O (4)
the polymethylene urea has the general formula: h2NCONH(CH2NHCONH)nH, wherein n is 1-10.
2. The method for preparing a compound fertilizer with a biological slow release function according to claim 1, wherein the type of the azotometer is KDN-08A, a certain amount of NaOH needs to be added when the temperature of the thermostatic waterbath is raised to 50 ℃ during the alkaline reaction in the step B, the reaction time is 2h, HPO is added during the acidic reaction in the step B, the temperature is kept unchanged at 50 ℃, and the reaction is terminated after the reaction time is 2 h.
3. The method for preparing a compound fertilizer with biological slow release function according to claim 1, wherein in the step D, the user dries at four temperature conditions of 80 ℃, 90 ℃, 100 ℃ and 110 ℃ for 2 hours respectively, measures the activity index of the product, compares to obtain a better drying temperature of the product, and then prepares the urea formaldehyde compound fertilizer with the best slow release effect.
4. The method for preparing a compound fertilizer with biological slow release function according to claim 1, wherein the temperature is controlled at 45-80 ℃ during the hydroxymethylation reaction, and the temperature is selected to be 45 ℃ by a user for reducing energy consumption, and the reaction time is 2.5 h.
5. The method for preparing a compound fertilizer with biological slow release function according to claim 1, wherein the temperature is maintained between 35 ℃ and 60 ℃ during the b-methylenation reaction, the temperature is selected by a user to be 40 ℃, and the reaction time is 2 h.
6. The method for preparing a compound fertilizer with biological slow release function according to claim 1, wherein the step a of hydroxymethylation is carried out under alkaline conditions, the pH value of alkaline solution is preferably 7-10, NaOH, K0H and Na2CO3All can be used for the pH value of the hydroxymethylation reaction, and NaOH is selected by a user.
7. The method for preparing a complex fertilizer with biological slow release function as claimed in claim 1, wherein the step b is performed under acidic condition during the methylenation reaction, and the pH value of the acidic solution is preferably controlled to 3-5, and the user can select phosphoric acid as the acidic solution because phosphoric acid can provide phosphorus necessary for crops, such as phosphoric acid, sulfuric acid, hydrochloric acid, etc.
CN201911374242.6A 2019-12-27 2019-12-27 Preparation method of compound fertilizer with biological slow release function Pending CN111138212A (en)

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Application publication date: 20200512