CS200671B1 - Process for preparing stable liquid phosphatic np-fertilizers - Google Patents
Process for preparing stable liquid phosphatic np-fertilizers Download PDFInfo
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- CS200671B1 CS200671B1 CS95078A CS95078A CS200671B1 CS 200671 B1 CS200671 B1 CS 200671B1 CS 95078 A CS95078 A CS 95078A CS 95078 A CS95078 A CS 95078A CS 200671 B1 CS200671 B1 CS 200671B1
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- Prior art keywords
- acid
- fertilizers
- fertilizer
- stable liquid
- liquid
- Prior art date
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- 239000003337 fertilizer Substances 0.000 title claims description 18
- 239000007788 liquid Substances 0.000 title description 11
- 238000004519 manufacturing process Methods 0.000 title description 5
- 239000002253 acid Substances 0.000 claims description 15
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- 238000006386 neutralization reaction Methods 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 230000003472 neutralizing effect Effects 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 claims description 2
- LRCFXGAMWKDGLA-UHFFFAOYSA-N dioxosilane;hydrate Chemical compound O.O=[Si]=O LRCFXGAMWKDGLA-UHFFFAOYSA-N 0.000 claims 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 12
- 239000000243 solution Substances 0.000 description 8
- 235000011007 phosphoric acid Nutrition 0.000 description 7
- 238000003860 storage Methods 0.000 description 5
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000004062 sedimentation Methods 0.000 description 4
- 239000010802 sludge Substances 0.000 description 4
- 239000012429 reaction media Substances 0.000 description 3
- 229910019142 PO4 Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000010924 continuous production Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- 235000021317 phosphate Nutrition 0.000 description 2
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 230000006641 stabilisation Effects 0.000 description 2
- 238000011105 stabilization Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 239000004114 Ammonium polyphosphate Substances 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 235000019826 ammonium polyphosphate Nutrition 0.000 description 1
- 229920001276 ammonium polyphosphate Polymers 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 235000021049 nutrient content Nutrition 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 150000003016 phosphoric acids Chemical class 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002522 swelling effect Effects 0.000 description 1
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- Fertilizers (AREA)
Description
Predmetom vynálezu je sposob přípravy stabilného kvapalného NP hnojivá ortofosforečnanováho typu.It is an object of the present invention to provide a method for preparing stable liquid NP fertilizers of the orthophosphate type.
Je známe, že pri neutrelizácii extrakčnej kyseliny trihydrofosforečnej amoniakom dochádza k zrážaniu fosforečnanov obsiahnutých v extrakčnej kyselině fosforečnéj, predovšetkým fosforečnanov Fe, AI, Mig, Ca vo formě gelovitej zrazeniny kalov, čo spósobuje určité tažkosti predovšetkým pri dlhodobejšom skladovaní kvapalných NP-hnojív, ako aj pri manipulácii a aplikácii.It is known that the neutralization of the extract of trihydrophosphoric acid with ammonia precipitates the phosphates contained in the extractive phosphoric acid, in particular the phosphates Fe, Al, Mig, Ca in the form of a gelled sludge precipitate, which causes some difficulties especially with prolonged storage of liquid NP-fertilizers handling and application.
Aby 8a zabránilo sedimentácii týchto kalov, přidávájl sa k NP-roztokom rožne stabilizujúce přísady, čo je predmetom celého radu patentov ( napr. USA patenty č. ),179.496, č. 3,160.495)· V prevažnej rniere sa v týchto výrobných postupoch využívají látky s tzv. napučiavacími vlastnostami, ktoré okrem toho, že podstatné znížia sedimentační rychlost jednotlivých častíc vyzrážaných kalov, sposobujl značné zvýšenie viskozity získaných produktov.In order to prevent sedimentation of these sludges, various stabilizing additives have been added to the NP solutions, which are the subject of a number of patents (e.g., U.S. Pat. In the production process, these substances use so called swelling properties which, in addition to substantially reducing the sedimentation rate of the individual particles of precipitated sludge, caused a considerable increase in the viscosity of the products obtained.
Nevýhodou týchto sposobov přípravy stabilných NP-hnojív je, že se v podstatě z finálneho roztokového hnojivá získává NP-suspenzné hnojivo, ktoré proti roztokovému hnojivu kladie ešte vyššie nároky na jeho skladovanie, transport a aplikáciu. Stabilizácia pornocou anarganických zlúčenin, obsahujících fosfor v kondenzovanéj formě ako sl PgO^, kondenzované fosforečné kyseliny a ich amonné, připadne alkalické kovy obsahujíce soli je predmetom US pat. č. 3,057.711.A disadvantage of these methods of preparing stable NP-fertilizers is that essentially the NP-slurry fertilizer is obtained from the final solution fertilizer, which places even greater demands on the solution fertilizer for its storage, transport and application. The stabilization of phosphorous-containing anarganic compounds in a condensed form such as s1 PgO4, condensed phosphoric acids and their ammonium or alkali metal containing salts is the subject of US Pat. no. 3,057.711.
200 071 Další spoaob stabilizácie aa uvádza v US pat. č. 3,661,897, podlá ktorého sa k výrobnému kvapalnému NP-hnojivu na báze polyfoaforečnanov amonných pridávajú zličeniny obsahujíce fluór, ako sú F a Sif| ’ .200 071 O ther spoaob and on the stabilization mentioned in U.S. Pat. no. 3,661,897, according to which fluorine-containing compounds such as F and Sif are added to the production liquid ammonium polyphosphate NP-fertilizer. '.
Terez se zlatilo, že stabilně kvapalné NP-hnojivo ortofosforečnanového typu možno s výhodou připravil neutralizáciou kyseliny trihydrofosforečnej plynným alobo kvapalným amoniakom alebo čpavkovou vodou, ak sa k trihydrofosforečnej kyselině před alebo v priebehu neutralizačně j reakcie Sálej přidá vodný roztok kyseliny fluorokremičitek v množstve Q,5 - 30 hmotových dielov 100 ž>-nej H^SiFg na 100 hmotových dielov UjPO^. Získá sa velmi stabilně kvapalné NP-hnojivo, ktoré si zachovává všetky vlastnosti roztokov a obsahuje tuhý podiel koloidne rozptýlený, nepodliehajúci počas skladovania stárnutiu tj. naraetaniu kryštálov. Ani po sedmi dňovom skladovaní nedochádza k vzniku čírek vrstvy roztoku, tj. k sedimentácii koloidne rozptýleného kalu. Takto získané NP-hnojivo ortofosforečnanového typu je možno bez komplikácií skladovat, transportovat i aplikoval podobné ako číře roztokové hnojivá.It has been gold-colored that a stably liquid orthophosphate-type NP fertilizer can be advantageously prepared by neutralizing trihydrophosphoric acid with gaseous alobo with liquid ammonia or ammonia water, if an aqueous solution of fluorosilicic acid is added to the trihydrophosphoric acid before or during the neutralization reaction. 30 parts by weight of 100% H 2 SiFg per 100 parts by weight of U 1 PO 4. A very stable liquid NP-fertilizer is obtained which retains all the properties of the solutions and contains a solid fraction colloidally dispersed, not subject to aging during storage, ie. crystals crystals. Even after seven days of storage, no clear layers of solution are formed, i. to sedimentation of colloidal dispersed sludge. The orthophosphate-type NP fertilizer thus obtained can be stored, transported and applied without any complications similar to pure fertilizer solutions.
Použitie HgSiFg je zvláši výhodné v případe kontinuálnych poetupov výroby kvapalných NP-hnojív, pretože teplota reakčného prostredia pri týchto postupoch je zvyčajne podstatné nižšia ako pri diskontinuálnych procesoch, takže nedochádza k rozkladu kyseliny fluorokremičitej a úniku fluorovodíka z reakčného prostredie. V zmysle vynálezu sa pri kontinuálnem spósobe výroby stabilného kvapalného NP-hnojiva ortofosforečnanového typu do reakčného priestoru privádza v potřebných množstvách osobitne H^PO^ a tígSiFg, ktoré sa súčaene neutralizuji plynným elebo kvapalným amonlakom alebo čpavkovou vodou alebo ea do reakčného prleetoru kontinuálně privádza tzv. zmesná kyselina obeahujúca H^PO^ a I^SiF^ v potřebných hmotových pomeroch (0,5 - 3θ % £-nej vztahovaná na 100 £-nú H^PO^). Týmto epoeobom sa získá stabilně kvapalné NP-hnojivo o požadovanom obsahu živin, o pH pohybujúcom sa v neutrálněj oblasti 6,0 - 7 a o nízkéj hodnotě dynamickéj viekozity.The use of HgSiFg is particularly advantageous in the case of continuous processes for the production of liquid NP-fertilizers, since the temperature of the reaction medium in these processes is usually substantially lower than in discontinuous processes so that decomposition of fluorosilicic acid and hydrogen fluoride escape from the reaction medium. According to the invention, in a continuous process for the production of a stable orthophosphate-type NP liquid fertilizer, the quantities of H 2 PO 4 and tigSiFg which are neutralized by gaseous or liquid ammonia or ammonia water are added to the reaction space. mixed acid containing H 2 PO 4 and I 2 SiF 3 in the necessary weight ratios (0.5-3% £ based on 100 nú H 3 PO ^). This epoeobom yields a stable liquid NP-fertilizer with the desired nutrient content, a pH in the neutral range of 6.0 - 7 and a low dynamic viscosity value.
Ďalej uvedené příklady ilustruji, ale nijako neobmedzuji predmet vynálezu.The following examples illustrate but do not limit the invention in any way.
Příklad 1Example 1
Zmesná kyselina sa připravila zmiešaním 414 g HgO, 1380 g extrakčnej kyseliny fosforečné j proveniencie Fosforico - ŠPANIELSKO obsahujicej 52,85 % 8 4,942 g 20,88 £-nej kyseliny fluorokremičitej, čo představuje 17,1 hmotových £ i^SiFg 100 £-nej z množstva 100 £-nej kyseliny trihydrogénfosforečnej. Kyselina trihydrogénfosforečná uvedemej proveniencie obsahuje podlá firemného atestu maximálně 0,45 % Fe20j * maximálně 0,45 % AlgO^ » maximálně 1,20 «Fa maximálně 3,5 % sír ano v. Zmesná kyselina sa počas 110 min|it dávkuje do kontinuálně pracujúceho reakčného systému v množstve 77,0 g min“^. Sičeene bole v množstve 46,0 g min“1 dávkované čpavková voda e obaahom 28,44 % NHj. Po 25 minitach kontinuálněj přípravy sa získalo 3 030 g kvapalného ortofosforečnanového NP-hnojiva vyznačujiceho sa vysokou stabilitou, takže v priebehu 14 dní skladovania nedoSlo k žiadnej sedimentácii koloidne rozptýleného kalu. Získaný produkt bol Specifikovaný následovně:The mixed acid was prepared by mixing 414 g of HgO, 1380 g of phosphoric acid of the provenance Fosforico - SPAIN containing 52.85% 8 of 4.942 g of 20.88% fluorosilicic acid representing 17.1% by weight of SiFg 100%. % of 100% orthophosphoric acid. Phosphoric acid contains provenance we state according to the company's certificate up to 0.45% Fe 2 0j * up to 0.45% Algo ^ »up to 1.20 'F a maximum of 3.5% in a broad, yes. The mixed acid was fed into the continuously operating reaction system at a rate of 77.0 g / min for 110 minutes. Sičeene bole in an amount of 46.0 g min "1 dosed kettle contents much ammonia water 28.44% N H. After 25 minutes of continuous preparation, 3030 g of liquid orthophosphate NP-fertilizer with high stability were obtained, so that no sedimentation of the colloidal dispersed sludge occurred during 14 days of storage. The product obtained was specified as follows:
- celkový obsah N : 8,50 £- Total N: £ 8.50
- celkový obsah P-,0^ : 22,93 £- total content of P 1 O 2: £ 22.93
200 67 obsah vodorozp. ·?2θ5 hodnotg pH roztoku marné hmotnost pri 20° óvnamif^é viskozita : 22,70 * : 6,5200 67 water content PH value of solution in vain weight at 20 ° viscosity: 22,70 *: 6,5
C : 1284 kg m-3 : 14,77 mPa.s /c?/C: 1284 kg m -3 : 14.77 mPa.s / c c /
Příklad 2Example 2
K příprava zmesnej kyseliny sa použilo 11 558 g extrakčnej kyseliny fosforečnej od holandské j firmy ttindmill o koncentraci! 52,08 % PgO^ a 4 942 g 20,88 /á-nej kyseliny fluorokremičitej, čo představuje 17,1 hmotových jfc H^SiF^ 100 Λ-nej z množstva 100 Λ-nej kyseliny trihydrogénfosforečnej. Počas 110 minút sa kontinuálně dávkovala do reakčného prostredia zmesná kyselina rýchlostou 145,64 g min~^ a súčasne čpavková voda obsahujúca 28,44 Λ NHj rýchlostou 74,1 g min”1·, pričom teplota reakčnej zmesi sa udržovala pri teplote 55° C. Celkom sa zadávkovalo 16 020 g zmesnej kyseliny a 8 151 g čpavkovéj vody. Vznikájúci produkt sa kontinuálně odobaral a získalo sa v celku 23 980 g stabilného kvapalného NP-hnojiva čo představovalo 99,2 %-ný výiažok.To prepare the mixed acid, 11,558 g of extract phosphoric acid from the Dutch company ttindmill were used at a concentration of 10%. 52.08% PgO 4 and 4.942 g of 20.88 g of fluorosilicic acid, representing 17.1 wt% of H 2 SiF 2 O, 100% of the amount of 100% orthophosphoric acid. Mixed acid was continuously metered into the reaction medium over a period of 110 minutes at a rate of 145.64 g min -1 and simultaneously ammonia water containing 28.44 Λ NH 3 at a rate of 74.1 g min -1 while maintaining the temperature of the reaction mixture at 55 ° C. In total, 16 020 g of mixed acid and 8 151 g of ammonia water were supplied. The resulting product was decolorized continuously and a total of 23,980 g of stable liquid NP-fertilizer was obtained, which represented a 99.2% yield.
Získaný produkt mal následovní! Špecifikéciu:The product obtained had the following! Špecifikéciu:
- celkový obsah Ntotal content
- celkový obsah ?2θ5- total content? 2θ5
- obsah vodorozp. ?2θ5- water content ? 2θ5
- hodnota ph roztoku- the pH value of the solution
- měrná hmotnost pri 20°- specific gravity at 20 °
- dynamická viskozita- dynamic viscosity
PŘEĎME' : 7,89 H>LOOK UP: 7.89 H>
: 24,08 A i 23,30 % : 6,1: 24.08 And 23.30%: 6.1
C : 1 318 kg m“3 : 15,34 mPa.s /cP/C: 1 318 kg m 3 : 15,34 mPa.s / cP /
Claims (1)
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS95078A CS200671B1 (en) | 1978-02-14 | 1978-02-14 | Process for preparing stable liquid phosphatic np-fertilizers |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS95078A CS200671B1 (en) | 1978-02-14 | 1978-02-14 | Process for preparing stable liquid phosphatic np-fertilizers |
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| Publication Number | Publication Date |
|---|---|
| CS200671B1 true CS200671B1 (en) | 1980-09-15 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CS95078A CS200671B1 (en) | 1978-02-14 | 1978-02-14 | Process for preparing stable liquid phosphatic np-fertilizers |
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| Country | Link |
|---|---|
| CS (1) | CS200671B1 (en) |
-
1978
- 1978-02-14 CS CS95078A patent/CS200671B1/en unknown
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