CN109438011A - Hydrochloric acid decomposes the method that lime stone prepares bulky grain nitrogenous fertilizer - Google Patents
Hydrochloric acid decomposes the method that lime stone prepares bulky grain nitrogenous fertilizer Download PDFInfo
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- CN109438011A CN109438011A CN201811457703.1A CN201811457703A CN109438011A CN 109438011 A CN109438011 A CN 109438011A CN 201811457703 A CN201811457703 A CN 201811457703A CN 109438011 A CN109438011 A CN 109438011A
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- China
- Prior art keywords
- cacl
- hydrochloric acid
- bulky grain
- nitrogenous fertilizer
- lime stone
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05C—NITROGENOUS FERTILISERS
- C05C3/00—Fertilisers containing other salts of ammonia or ammonia itself, e.g. gas liquor
Abstract
The invention discloses a kind of hydrochloric acid to decompose the method that lime stone prepares bulky grain nitrogenous fertilizer, comprising the following steps: 1) mixes hydrochloric acid with lime stone and react, then filter, filtrate is spare；2) filtrate is flashed to obtain CaCl2Solution, CaCl2Solution is delivered to multistage evaporation system and is evaporated, and obtains CaCl2Supersaturated solution；3) CaCl2Supersaturated solution send to vacuum filter, obtain wet CaCl2Crystal, then be dried to obtain anhydrous CaCl2；4) by anhydrous CaCl2With ammonium sulfate and urea together as raw material, 3-5:60-90:8-35 in mass ratio is granulated, and bulky grain nitrogenous fertilizer is made.The present invention is with anhydrous CaCl2For binder, the bulky grain nitrogenous fertilizer prepared by pellet granulation, while the ammonium sulfate containing ammonium nitrogen and the urea with amidonitrogen is added, compared to the nitrogen of more single form, the more conducively growth of crops.And it is raw material using industrial waste hydrochloric acid and caprolactam by-product ammonium sulfate, produces bulky grain nitrogenous fertilizer, realizes recycling for resource.
Description
Technical field
The present invention relates to technical field of fertilizers, and in particular to a kind of hydrochloric acid decomposition lime stone prepares the side of bulky grain nitrogenous fertilizer
Method.
Background technique
During domestic mortar gunite method production S-based compound fertilizer, a large amount of hydrochloric acid of by-product, currently, without effective reliable method
It is used, enterprise needs to spend to be handled instead, seriously constrains the development of S-based compound fertilizer.Similarly, ammonium sulfate is
By-product in caprolactam production process, amount is big and is difficult to digest, and is used, turns waste into wealth to these wastes and by-product,
Recycling for resource can not only be promoted, the performance of enterprises can also be increased.
Summary of the invention
In order to solve the above technical problem, the present invention provides a kind of hydrochloric acid to decompose the side that lime stone prepares bulky grain nitrogenous fertilizer
Method can produce high-quality bulky grain nitrogenous fertilizer using cheap raw material.
The technical solution adopted by the present invention is that a kind of method that hydrochloric acid decomposition lime stone prepares bulky grain nitrogenous fertilizer, including with
Lower step:
1) hydrochloric acid is mixed with lime stone and is reacted, then filtered, filtrate is spare；
2) filtrate is flashed to obtain CaCl2Solution, CaCl2Solution is delivered to multistage evaporation system and is evaporated, and obtains CaCl2
Supersaturated solution；
3) CaCl2Supersaturated solution send to vacuum filter, obtain wet CaCl2Crystal, then be dried to obtain anhydrous CaCl2；
4) by anhydrous CaCl2With ammonium sulfate and urea together as raw material, 3-5:60-90:8-35 in mass ratio is granulated, system
Obtain bulky grain nitrogenous fertilizer.
Further, the hydrochloric acid is dilute hydrochloric acid or concentrated hydrochloric acid.
Further, the hydrochloric acid is the hydrochloric acid that mortar gunite method produces S-based compound fertilizer by-product.
Further, the ratio between hydrogen chloride and the amount of substance of calcium carbonate in lime stone are 2.0-2.5 in hydrochloric acid in step 1):
1。
Further, reaction temperature is 20-50 DEG C in step 1), reaction time 20-60min.
Further, the HCl gas evaporated in flash process in step 2, which returns in step 1), continues to participate in reaction.
Further, multistage evaporation system described in step 2 is three-level, steam and CaCl2Solution inversely contacts,
Middle level-one evaporator temperature is 200-300 DEG C, and secondary evaporimeter temperature is 300-400 DEG C, and three-level evaporator temperature is 400-500
℃。
Further, ammonium sulfate described in step 4) is caprolactam by-product.
Further, it when being granulated in step 4), is granulated using granulating method.
The invention further relates to the bulky grain nitrogenous fertilizer being prepared using the method.Including following original by weight
Material: the mixing of all raw materials is carried out being granulated greatly by CaCl23-5 part anhydrous, 60-90 parts of ammonium sulfate and 8-35 parts of urea, when preparation
Particle nitrogen fertilizer.
The partial size of the bulky grain nitrogenous fertilizer is 2-4mm.
The present invention has the following advantages that and effect:
1, the use of industrial waste hydrochloric acid and caprolactam by-product ammonium sulfate is raw material, produces bulky grain nitrogenous fertilizer, turn waste into wealth,
Be conducive to environmental protection, while solving the problems, such as how enterprise handles trade waste, realize recycling for resource, generates
Good economic benefit.
2, hydrochloric acid decomposes the anhydrous CaCl that lime stone generates2With extensive industrial use, it can be used as desiccant, refrigeration
Agent, antifreezing agent, deicing salt, antifogging agent and road surface dust-collecting agent etc., the present invention in anhydrous CaCl2For binder, pass through granulating method
It is granulated the bulky grain nitrogenous fertilizer of preparation, while the ammonium sulfate containing ammonium nitrogen and the urea with amidonitrogen is added, compared to more single
The nitrogen of form, the more conducively growth of crops.
Specific embodiment
Below with reference to embodiment, the present invention is furture elucidated.
Embodiment 1:
Lime stone and technical hydrochloric acid are proportionally added into mixing channel, hydrogen chloride and carbon in lime stone in the hydrochloric acid of addition are controlled
The ratio between amount of substance of sour calcium be 2.5:1, the reaction time 30 minutes, 50 DEG C of reaction temperature.Slurry sufficiently after reaction carried out
Filter is obtained containing CaCl2Supernatant, filtrate is flashed, the HCl gas that evaporates returns to mixing channel, obtains main component
For CaCl2Solution, by its with pump be delivered to multistage evaporation system, wherein level-one evaporator temperature be 250 DEG C, secondary evaporimeter
Temperature is 350 DEG C, and three-level evaporator temperature is 500 DEG C, and CaCl is obtained after multistage evaporation2Supersaturated solution, then will
CaCl2Supersaturated solution pump is delivered to vacuum type belt filter, filters out most of moisture, obtains wet CaCl2Crystal, then pass through
It crosses and is dried to obtain solid water-free CaCl2。
The anhydrous CaCl that will be produced2, with ammonium sulfate and urea together as raw material, addition carries out granulating method rotary drum in proportion
It is granulated, wherein anhydrous CaCl24% is accounted for, ammonium sulfate accounts for 88%, and urea accounts for 8%, and bulky grain nitrogenous fertilizer is made.
Obtained bulky grain nitrogenous fertilizer is detected, and N22%, moisture 0.8%, average particle size 2.5mm are contained.
Embodiment 2:
Lime stone and technical hydrochloric acid are proportionally added into mixing channel, hydrogen chloride and carbon in lime stone in the hydrochloric acid of addition are controlled
The ratio between amount of substance of sour calcium be 2.2:1, the reaction time 50 minutes, 40 DEG C of reaction temperature.Slurry sufficiently after reaction carried out
Filter is obtained containing CaCl2Supernatant, filtrate is flashed, the HCl gas that evaporates returns to mixing channel, obtains main component
For CaCl2Solution, by its with pump be delivered to multistage evaporation system, wherein level-one evaporator temperature be 280 DEG C, secondary evaporimeter
Temperature is 375 DEG C, and three-level evaporator temperature is 500 DEG C, and CaCl is obtained after multistage evaporation2Supersaturated solution, then will
CaCl2Supersaturated solution pump is delivered to vacuum type belt filter, filters out most of moisture, obtains wet CaCl2Crystal, then pass through
It crosses and is dried to obtain solid water-free CaCl2。
The anhydrous CaCl produced2, with ammonium sulfate and urea together as raw material, addition progress granulating method rotary drum is made in proportion
Grain, wherein anhydrous CaCl25% is accounted for, ammonium sulfate accounts for 80%, and urea accounts for 15%, and bulky grain nitrogenous fertilizer is made.
Obtained bulky grain nitrogenous fertilizer is detected, and N23.5%, moisture 0.67%, average particle size 2.4mm are contained.
Embodiment 3:
Lime stone and technical hydrochloric acid are proportionally added into mixing channel, hydrogen chloride and carbon in lime stone in the hydrochloric acid of addition are controlled
The ratio between the amount of substance of sour calcium is the reaction time 40 minutes, 45 DEG C of reaction temperature.Slurry sufficiently after reaction is filtered, and is obtained
To containing CaCl2Supernatant, filtrate is flashed, the HCl gas that evaporates returns to mixing channel, and obtaining main component is CaCl2
Solution, it is delivered to multistage evaporation system with pump, wherein level-one evaporator temperature is 270 DEG C, and secondary evaporimeter temperature is
340 DEG C, three-level evaporator temperature is 500 DEG C, and CaCl is obtained after multistage evaporation2Supersaturated solution, then by CaCl2Satiety
It is delivered to vacuum type belt filter with solution pump, most of moisture is filtered out, obtains wet CaCl2Crystal, drying obtain
To solid water-free CaCl2。
The anhydrous CaCl that will be produced2, with ammonium sulfate and urea together as raw material, addition carries out granulating method rotary drum in proportion
It is granulated, wherein anhydrous CaCl23% is accounted for, ammonium sulfate accounts for 67%, and urea accounts for 30%, and bulky grain nitrogenous fertilizer is made.
Obtained bulky grain nitrogenous fertilizer is detected, and N27.7%, moisture 0.75%, average particle size 2.7mm are contained.
Comparative example:
Calcium nitrate (or calcium sulfate) is mixed with ammonium sulfate and urea 3:67:30 in mass ratio, using granulating method rotary drum
It is granulated, is unable to get large-particle fertilizer.
The above embodiments are only the preferred technical solution of the present invention, and are not construed as limitation of the invention, this hair
Bright protection scope should be with the technical solution of claim record, technical characteristic in the technical solution recorded including claim
Equivalents are protection scope.Equivalent replacement i.e. within this range is improved, also within protection scope of the present invention.
Claims (10)
1. a kind of hydrochloric acid decomposes the method that lime stone prepares bulky grain nitrogenous fertilizer, which comprises the following steps:
1) hydrochloric acid is mixed with lime stone and is reacted, then filtered, filtrate is spare；
2) filtrate is flashed to obtain CaCl2Solution, CaCl2Solution is delivered to multistage evaporation system and is evaporated, and obtains CaCl2
Supersaturated solution；
3) CaCl2Supersaturated solution send to vacuum filter, obtain wet CaCl2Crystal, then be dried to obtain anhydrous CaCl2；
4) by anhydrous CaCl2With ammonium sulfate and urea together as raw material, 3-5:60-90:8-35 in mass ratio is granulated, system
Obtain bulky grain nitrogenous fertilizer.
2. according to the method described in claim 1, it is characterized by: the hydrochloric acid is dilute hydrochloric acid or concentrated hydrochloric acid.
3. according to the method described in claim 1, it is characterized by: the hydrochloric acid is that mortar gunite method produces S-based compound fertilizer by-product
Hydrochloric acid.
4. according to the method described in claim 1, it is characterized by: calcium carbonate in hydrogen chloride and lime stone in hydrochloric acid in step 1)
The ratio between the amount of substance be 2.0-2.5:1.
5. according to the method described in claim 1, it is characterized by: in step 1) reaction temperature be 20-50 DEG C, the reaction time
20-60min。
6. according to the method described in claim 1, it is characterized by: the HCl gas evaporated in flash process in step 2 returns
Reaction is continued to participate in into step 1).
7. according to the method described in claim 1, it is characterized by: multistage evaporation system described in step 2 is three-level, steaming
Vapour and CaCl2Solution inversely contacts, and wherein level-one evaporator temperature is 200-300 DEG C, and secondary evaporimeter temperature is 300-400
DEG C, three-level evaporator temperature is 400-500 DEG C.
8. according to the method described in claim 1, it is characterized by: ammonium sulfate described in step 4) is caprolactam by-product
Object.
9. according to the method described in claim 1, it is characterized by: being granulated when being granulated in step 4) using granulating method.
10. a kind of bulky grain nitrogenous fertilizer, which is characterized in that including following raw material by weight: anhydrous CaCl23-5 parts, sulfuric acid
60-90 parts of ammonium and 8-35 parts of urea, when preparation, which mixes all raw materials, to carry out being granulated to obtain bulky grain nitrogenous fertilizer.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111960894A (en) * | 2020-08-26 | 2020-11-20 | 山西绿丰肥业有限公司 | Water-soluble fertilizer capable of quickly improving nutrients of crops and preparation method thereof |
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|---|---|---|---|---|
| GB401788A (en) * | 1932-04-27 | 1933-11-23 | American Cyanamid Co | A process for preparing stable granulated calcium cyanamide |
| GB990722A (en) * | 1961-05-30 | 1965-04-28 | Centre Nat Rech Metall | Fertilizer production |
| CN101683997A (en) * | 2008-09-26 | 2010-03-31 | 天津市黎虹化工有限公司 | Method for producing calcium chloride dihydrate |
| CN102826893A (en) * | 2011-11-25 | 2012-12-19 | 中国科学院烟台海岸带研究所 | Organic-inorganic compound fertilizer binder and its preparation method |
| CN104262007A (en) * | 2014-09-29 | 2015-01-07 | 高台县旺达绿禾肥业有限责任公司 | Whole water-soluble nitrogen fertilizer with relatively high pelletizing rate |
| CN104773750A (en) * | 2015-03-25 | 2015-07-15 | 聊城市鲁西化工工程设计有限责任公司 | System for producing anhydrous calcium chloride by using industrial waste hydrochloric acid, and technology thereof |
| CN104995133A (en) * | 2013-03-29 | 2015-10-21 | 大曹株式会社 | Tablet for preparing solution of chlorine dioxide |
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| CN107117992A (en) * | 2017-06-12 | 2017-09-01 | 贵州诺威施生物工程有限公司 | Calcium chloride preparation system and calcium chloride preparation method |
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| GB401788A (en) * | 1932-04-27 | 1933-11-23 | American Cyanamid Co | A process for preparing stable granulated calcium cyanamide |
| GB990722A (en) * | 1961-05-30 | 1965-04-28 | Centre Nat Rech Metall | Fertilizer production |
| CN101683997A (en) * | 2008-09-26 | 2010-03-31 | 天津市黎虹化工有限公司 | Method for producing calcium chloride dihydrate |
| CN102826893A (en) * | 2011-11-25 | 2012-12-19 | 中国科学院烟台海岸带研究所 | Organic-inorganic compound fertilizer binder and its preparation method |
| CN104995133A (en) * | 2013-03-29 | 2015-10-21 | 大曹株式会社 | Tablet for preparing solution of chlorine dioxide |
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| CN105906356A (en) * | 2016-04-25 | 2016-08-31 | 中国工程物理研究院材料研究所 | Method for preparing high-purity hydration-resisting calcium oxide crucible |
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|---|---|---|---|---|
| CN111960894A (en) * | 2020-08-26 | 2020-11-20 | 山西绿丰肥业有限公司 | Water-soluble fertilizer capable of quickly improving nutrients of crops and preparation method thereof |
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Application publication date: 20190308 |