CN103073347B - Long-term-stability and synergistic ammonium chloride fertilizer with combined-soda process, and preparation method thereof - Google Patents
Long-term-stability and synergistic ammonium chloride fertilizer with combined-soda process, and preparation method thereof Download PDFInfo
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- CN103073347B CN103073347B CN201110330391.XA CN201110330391A CN103073347B CN 103073347 B CN103073347 B CN 103073347B CN 201110330391 A CN201110330391 A CN 201110330391A CN 103073347 B CN103073347 B CN 103073347B
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- 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
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Abstract
The invention relates to a long-term fertilizer and a preparation method thereof, and specifically a long-term-stability and synergistic ammonium chloride fertilizer and a preparation method thereof. According to the invention, ammonium chloride crystallized from cold precipitation and salting in a process for producing soda ash with a combined-soda process is mixed with the added ammonium stabilizer and/or synergist before entering a separation and drying process. The fertilizer comprises ammonium chloride, an ammonium stabilizer, and/or a synergist. According to the weight, ammonium chloride: ammonium stabilizer: synergist=1:0.001-0.1:0.0001-0.05; ammonium chloride: ammonium stabilizer=1:0.001-0.1. The ammonium chloride is a by-product ammonium chloride obtained in a process for producing soda ash with a combined-soda process. The long-term or stable/synergistic ammonium chloride fertilizer preparation method has the advantages of process saving, low cost, high quality, and stable effect. With the method, the long-term or stable/synergistic ammonium chloride has the advantages of uniform texture and stable effect. Nitrogen utilization rate of ammonium chloride is improved by 10-20 percentage points, and ammonium chloride utilization amount is reduced by more than 50%. Ammonium chloride fertilizer effect time is prolonged from 20-30 days to 80-100 days. After one time of fertilizing, top dressing can be avoided.
Description
Technical field
The present invention relates to production controlled availability fertilizer, one utilizes union soda device production long-term stability, synergy ammonium chloride fertilizer and preparation method specifically.
Background technology
Union soda (also known as Hou's process for soda production) is the complete industrial alkaline (Na proposed China's famous chemist Houde Bang nineteen forty-two
2cO
3) method.Within 1961, building up China's First connection alkali workshop in Dalian, afterwards through improving and development, having become now major technique pillar and the method for basic industry.Union soda raw material availability is high, and wherein the utilization ratio of NaCl reaches more than 90%, and do not need Wingdale, coke (coal), fuel economy, raw material, the energy and trucking costs, make product cost decline to a great extent.Do not need ammonia still, limestone kiln, the Large heavy equipment such as lime slaking machine, shorten flow process, reduce investment outlay, do not produce the discharge of a large amount of waste residue and liquid, it is harsh that factory site of founding the factory requires do not have solvay soda process.Therefore the main method of basic industry is up to the present remained.
hou's process for soda productionprinciple be foundation
ionic reactionthe principle occurred is carried out, and the direction that ionic reaction can reduce towards ionic concn is carried out.Soda ash (Na processed
2cO
3), first utilize NaHCO
3the less obtained NaHCO of solubleness in solution in the solution
3.The decomposition of recycling sodium bicarbonate unstable obtains soda ash.In saturated aqueous common salt, pass into ammonia, form saturated ammonia salt solution, then pass into carbonic acid gas wherein, the first step is
ammoniawith water and
carbonic acid gasreaction generates a part
bicarbonate of ammonia; Second step be bicarbonate of ammonia with
sodium-chlorreaction generates a part
ammonium chloridewith
sodium bicarbonateprecipitation, sodium bicarbonate
solublenessless and Precipitation.According to NH
4the solubleness of Cl when normal temperature is larger than NaCl, and principle less than NaCl solubleness at low temperatures, when 278K ~ 283K (5 DEG C ~ 10 DEG C), add in mother liquor
saltfine powder, and make NH
4the independent crystallization of Cl.Therefore another product that union soda is produced is exactly NH
4cl is white crystal, theoretical containing N
2amount is 26.2%, can do
nitrogenous fertilizer.
Technologically, combined soda method legal system soda ash and Production of Ammonium Chloride.Be divided into two processes, the first process is soda manufacture process, and the second process is Production of Ammonium Chloride process, and two processes form a circulation.In the recycle system, add raw material ammonia, salt (sodium-chlor) and carbonic acid gas continuously, constantly produce soda ash and ammonium chloride product simultaneously.The mother liquor II that alkali producing process i.e. the second process is come inhales ammonia becomes ammonia mother liquor II, in carbonating tower, pass into carbonic acid gas and cool, that sodium-chlor in wooden leaf and ammonium salt (ammonia, carbonic acid gas, water react) change into sodium bicarbonate and ammonium chloride, then sodium bicarbonate crystallization is leached, again send into calcining soda ash, the mother liquor leached becomes mother liquor I.Its each portion net reaction is respectively:
NH
3+ NaCl+CO
2+ H
2o → NaHCO
3↓+NH
4cl (carburizing reagent)
2NaHCO
3→ NaCO
3+ CO
2↑+H
2o ↑ (calcining)
Production of Ammonium Chloride process is that the ammonia mother liquor I generated after the mother liquor I of I process is inhaled ammonia cools, and makes it to separate out ammonium chloride; Then add salt, make ammonium chloride continue to separate out by means of common-ion effcet, then separated by crystallization ammonium chloride, the mother liquor leached becomes mother liquor II, is recycled to I process alkaline and uses.The wet ammonium chloride filtered out send packaging after drying.
NH
4cl proportion 1.532, solution heat is 16.73kJ/mol, is heated to 400 DEG C of fusings at air tight condition, starts distillation, be decomposed into NH when 337.8 DEG C when being heated to 100 DEG C in atmosphere
3and HCl.NH
4the easy moisture absorption caking of Cl, brings certain difficulty to storage transport.NH
4cl is a kind of good nitrogen fertilizer in agriculture, and particularly suitable produces compound manure.
Current China chloride yield is steady growth situation: 2005 6030000 tons, 2006 6240000 tons, 2007 7250000 tons, 2008 8600000 tons, 2009 9180000 tons.Within 2010, chloride yield is close to 1,000 ten thousand tons.The proportion of ammonium chloride in China's nitrogenous fertilizer output by 2005 4% bring up to present more than 6%.
Ammonium chloride is ammonium fertilizer, ammonium chloride is unstable as common nitrogenous fertilizer nitrogen, after being manured into soil, easily producing ammonia volatilization and be converted into nitric nitrogen and run off, strong nitrification and denitrification effect occurs, a large amount of nitrogen nutrition is caused to run off, fertilizer efficiency period is short, and nitrogen utilization efficiency only has 15-20%, and nitrogen utilization efficiency is low, not only cause resource and economic significant wastage, also pollution (waters, air etc.) is caused to ecotope simultaneously.Use common ammonium chloride need repeatedly topdress, so not only wasted manure resources but also increased amount transport and labour cost, therefore market outlook allow of no optimist.
Utilize union soda production technique to produce the enterprise of soda ash much in China and even countries in the world, the ammonium chloride of China is almost all produced, so the exploitation of ammonium chloride directly have influence on again the sound development of Lian Jian enterprise of China from connection alkali.Soda ash is widely used in the industrial sectors such as building materials, light industry, chemical industry, metallurgy, weaving and daily life, and people can be rated as soda industry for " mother of chemical industry ".Therefore, develop long-acting ammonium chloride, improve the nitrogen utilization efficiency of ammonium chloride, for the agriculture production of promotion China, the industry of stable connection alkali, preserve the ecological environment all very important.
Summary of the invention
One is the object of the present invention is to provide to utilize union soda device production long-term stability, synergy ammonium chloride fertilizer and preparation method.
For achieving the above object, the technical solution used in the present invention is:
One utilizes union soda device production long-term stability, synergy ammonium chloride fertilizer: fertilizer component is ammonium chloride, ammonium stablizer and/or synergistic agent; Count by weight, wherein ammonium chloride: ammonium stablizer: synergistic agent=1: 0.001-0.1: 0.0001-0.05; Ammonium chloride: ammonium stablizer=1: 0.001-0.1; Wherein ammonium chloride is utilize the by-product ammonium chloride in union soda production soda ash technique.
Described inhibitor is Dyhard RU 100,3; 4-dimethyl pyrazole phosphoric acid salt, 3; 5-dimethyl pyrazole, 3; 5-dimethyl pyrazole phosphoric acid salt, 1-methylamine acyl group-3-methylpyrazole, 1-methylpyrazole-1 carboxylic acid amides, 3-methylpyrazole, nitrogen-pyridine (the chloro-6-of 2-(trichloromethyl)-pyridine) (code name CP; commodity are called N-Serve), or one or more in the chloro-3-methylpyrazole of 4-.
Described synergistic agent is poly-aspartic-acid (PASP) and salt thereof.Described synergistic agent is molecular weight: 6001 ~ 100000, structural formula such as formula 1 poly-aspartic-acid and salt, or be molecular weight: 2000 ~ 6000, structural formula such as formula 2 poly-aspartic-acid and salt.
Formula 1
Formula 2.
Utilize the preparation method of union soda device production long-term stability, synergy ammonium chloride fertilizer: add ammonium stablizer in the by-product ammonium chloride of producing in soda ash technique in union soda by weight proportion and/or synergistic agent is dissolved in carrier, puddled evenly by mixing pump machinery or after hand mixing, namely obtain long-term stability, synergy ammonium chloride fertilizer.Described carrier is formaldehyde, methyl alcohol, ethanol, ether, chloroform, methylene dichloride or tetracol phenixin.
In union soda production soda ash technique, cold analysis and salting-out crystallization ammonium chloride out mix with interpolation ammonium stablizer and/or synergistic agent before entering and being separated drying.
The principle of the invention: produce on the process for producing chloride basis in soda ash technique in former union soda, add the dosing unit of ammonium stablizer and/or synergistic agent, storage device and metering device system, in former union soda production soda ash technique, cold analysis and salting-out crystallization ammonium chloride out add ammonium stablizer and/or synergistic agent before entering and being separated drying installation, make added inhibitor and ammonium chloride realize being mixed fully in drying process, complete the production process of long-acting or stable/synergy ammonium chloride.
Institute of the present invention tool has the following advantages:
1. province's operation, cost is low.The present invention produces in the technique of soda ash after soda ash is separated out in union soda, ammonium chloride product produce dry before add the ammonium chloride nitrogen manure that long-acting or stable/synergy made by ammonium stablizer and/or synergistic agent in operation.Utilizing union soda to produce soda ash process system direct production, without the need to adding ammonium stablizer and/or synergistic agent again by after finished product chloride leach again, economizing operation, cost-saving.
2. high, the effect stability of quality.The present invention adds before last procedure to add ammonium stablizer and/or synergistic agent in process for producing chloride, now ammonium chloride is not also dried to solid particulate, this makes added ammonium stablizer and/or synergistic agent can fully and ammonium chloride molecule or Ar ion mixing, ensure that long-acting or stable/synergy ammonium chloride is homogeneous, effect stability.Overcome the unhomogeneity shortcoming that the usual ammonia chloride crystal generally adopted mixes with ammonium stablizer;
3. reduce rate of fertilizer application.The present invention obtains fertilizer and improves nitrogen utilization efficiency 10-20 percentage point in ammonium chloride, reduces ammonium chloride usage quantity more than 50%;
4. extend fertilizer efficiency period.The ammonium chloride fertilizer efficiency period that the present invention obtains extended to 80-100 days from 20-30 days, realized single-dose application and exempted to topdress;
5. fertilizer of the present invention promotes that plant utilizes other Nutrient Absorption, has the growth promoting root system, healthy and strong plant, significantly strengthens disease-resistant, drought resisting, precocity effect resistant to lodging and short;
6. increase crop yield.Within the scope of crop yield potentiality, etc. nitrogen quantity fertilising, crop yield can be improved at more than 8-10%.
7. improve crop quality, improve commercial grade.Significantly can improve crop product quantity.
Accompanying drawing explanation
The process flow sheet that Fig. 1 provides for the embodiment of the present invention.
Embodiment:
Below in conjunction with embodiment, the invention will be further described.
Produce in soda ash technique with former union soda and produce on byproduct process for producing chloride basis, utilize union soda to produce soda ash process unit system and carry out the long-acting or stable chlorination ammonium fertilizer of production.
Embodiment 1
Utilize union soda to produce soda ash technique, produce containing the long-acting ammonium chloride fertilizer of Dyhard RU 100, see Fig. 1:
In 100 parts of (quality) ammonium chlorides, add 1 part of Dyhard RU 100.
Dyhard RU 100 is added in the formaldehyde solution of mass percent 37% and fully dissolve in dosing unit, then be stored in storage device, utilize dosing device system, as volume pump, by dicyandiamide solution with produce in former union soda cold analysis and salting-out crystallization ammonium chloride out in soda ash technique enter be separated drying installation before fully mix, dry through being separated, i.e. obtained long-acting or stability ammonium chloride fertilizer.
Embodiment 2:
Produce in soda ash technique in union soda, produce containing 3,4-dimethyl pyrazole phosphoric acid salt and poly-aspartic-acid (PASP) long-acting added-acting ammonium chloride fertilizer:
In 100 parts of (quality) ammonium chlorides, add 0.5 part of 3,4-dimethyl pyrazole phosphoric acid salt, 0.3 part of poly-aspartic-acid (PASP).
By 3, 4-dimethyl pyrazole phosphoric acid salt and molecular weight be 10000 poly-aspartic-acid (PASP) add water, fully dissolve in dosing unit in the formaldehyde of mass percent 37% or the ethanolic soln of mass percent 95%, then be stored in storage device, utilize dosing device system, as volume pump, by 3, 4-dimethyl pyrazole phosphoric acid salt and poly-aspartic-acid (PASP) with produce in former union soda cold analysis and salting-out crystallization ammonium chloride out in soda ash technique enter be separated drying installation before fully mix, dry through being separated, i.e. obtained long-acting or stability ammonium chloride fertilizer.
Embodiment 3:
In 100 parts of (quality) ammonium chlorides, add 1 part of nitrogen-pyridine, 0.6 part of molecular weight is 20000 poly-aspartic-acids (PASP) sodium salt.
Nitrogen-pyridine and poly-aspartic-acid (PASP) sodium salt are added in the formaldehyde of mass percent 37%, ethanolic soln or water and fully dissolve in dosing unit, then be stored in storage device, utilize dosing device system, as volume pump, by nitrogen-pyridine and poly-aspartic-acid (PASP) sodium salt with produce in former union soda cold analysis and salting-out crystallization ammonium chloride out in soda ash technique enter be separated drying installation before fully mix, dry through being separated, i.e. obtained long-acting or stability ammonium chloride fertilizer.
Embodiment 4:
In 100 parts of (quality) ammonium chlorides, add 2 parts of Dyhard RU 100s, 0.5 part of 3,4-dimethyl pyrazole phosphoric acid salt.
By Dyhard RU 100,3,4-dimethyl pyrazole phosphoric acid salt adds mass percent 37% and (fully dissolves in dosing unit in formaldehyde, ethanolic soln or water, then be stored in storage device, utilize dosing device system, as volume pump, by Dyhard RU 100,3,4-dimethyl pyrazole phosphoric acid salt mixing solutions with produce in former union soda cold analysis and salting-out crystallization ammonium chloride out in soda ash technique enter be separated drying installation before fully mix, dry through being separated, i.e. obtained long-acting or stability ammonium chloride fertilizer.
5. embodiment 5:
In 100 parts of (quality) ammonium chlorides, add 1 part of Dyhard RU 100,0.1 part of nitrogen-pyridine and 1 part of molecular weight are 12000 poly-aspartic-acids (PASP).
Dyhard RU 100, nitrogen-pyridine and poly-aspartic-acid are added in the formaldehyde of mass percent 37%, ethanolic soln or water and fully dissolve in dosing unit, then be stored in storage device, utilize dosing device system, as volume pump, by Dyhard RU 100, nitrogen-pyridine and poly-aspartic-acid mixing solutions with produce in former union soda cold analysis and salting-out crystallization ammonium chloride out in soda ash technique enter be separated drying installation before fully mix, dry through being separated, i.e. obtained long-acting or stability ammonium chloride fertilizer.
Application examples:
The fertilizer effect on corn utilizing embodiment 2 to produce:
Effect test 1:
Varieties of plant used is new Dongdan 90.Mu executes embodiment 2 made fertilizer purity nitrogen 12kg, and common ammonium chloride purity nitrogen 15kg is executed in contrast, once makees base fertilizer and applies.Application effect is as shown in table 1.
Table 1 reduces the test effect of rate of fertilizer application
| Fertilizer | Corn per mu yield kg | Volume increase % | Save fertile % |
| Common ammonium chloride | 623 | 0.00 | 0.00 |
| Long-acting ammonium chloride | 645 | 3.53 | 20.00 |
Effect test 2
Varieties of plant used is new Dongdan 90.Mu executes embodiment 2 made fertilizer purity nitrogen 12kg, and common ammonium chloride purity nitrogen 12kg is executed in contrast, once makees base fertilizer and applies.Application effect is as shown in table 2.
The test effect of the identical fertilise of table 2.
| Fertilizer | Corn per mu yield kg | Volume increase % | Save fertile % |
| Common ammonium chloride | 565 | 0.00 | 0.00 |
| Long-acting ammonium chloride | 634 | 12.21 | 0.00 |
Claims (1)
1. the long-term stability utilizing union soda device to produce, a synergy ammonium chloride fertilizer, is characterized in that: fertilizer component is ammonium chloride, ammonium stablizer and synergistic agent; Count by weight, wherein ammonium chloride: ammonium stablizer: synergistic agent=1: 0.001-0.1: 0.0001-0.05; Ammonium chloride: ammonium stablizer=1: 0.001-0.1; Wherein ammonium chloride is utilize the by-product ammonium chloride in union soda production soda ash technique;
Described ammonium stablizer is Dyhard RU 100,3,4-dimethyl pyrazole phosphoric acid salt, 3, one or more in 5-dimethyl pyrazole, 3，5-dimethylpyrazole phosphoric acid salt, 1-methylamine acyl group-3-methylpyrazole, 1-methylpyrazole-1-carboxylic acid amides, 3-methylpyrazole, nitrogen-pyridine (the chloro-6-of 2-(trichloromethyl)-pyridine) or the chloro-3-methylpyrazole of 4-;
Described synergistic agent is molecular weight: 6001 ~ 100000, structural formula such as formula 1 poly-aspartic-acid and salt, or be molecular weight: 2000 ~ 6000, structural formula such as formula 2 poly-aspartic-acid and salt
Add ammonium stablizer in the by-product ammonium chloride of producing in soda ash technique in union soda by weight proportion and synergistic agent is dissolved in carrier, puddled evenly by mixing pump machinery or after hand mixing, namely obtain long-term stability, synergy ammonium chloride fertilizer;
In union soda production soda ash technique, cold analysis and salting-out crystallization ammonium chloride out mix with interpolation ammonium stablizer and synergistic agent before entering and being separated drying;
Described carrier is formaldehyde, methyl alcohol, ethanol, ether, chloroform, methylene dichloride or tetracol phenixin.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1204631A (en) * | 1998-07-10 | 1999-01-13 | 寇庆德 | Nitrogenous fertilizer long-acting synergist |
| CN101434502A (en) * | 2007-11-16 | 2009-05-20 | 中国科学院沈阳应用生态研究所 | Synergistic slow release nitrogen fertilizer and preparation thereof |
| CN101844948A (en) * | 2010-05-17 | 2010-09-29 | 山东省农业科学院土壤肥料研究所 | Use of natural azadirachtin plant material as nitrogen fertilizer synergist |
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2011
- 2011-10-26 CN CN201110330391.XA patent/CN103073347B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1204631A (en) * | 1998-07-10 | 1999-01-13 | 寇庆德 | Nitrogenous fertilizer long-acting synergist |
| CN101434502A (en) * | 2007-11-16 | 2009-05-20 | 中国科学院沈阳应用生态研究所 | Synergistic slow release nitrogen fertilizer and preparation thereof |
| CN101844948A (en) * | 2010-05-17 | 2010-09-29 | 山东省农业科学院土壤肥料研究所 | Use of natural azadirachtin plant material as nitrogen fertilizer synergist |
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