DE1024934B - Process for the production of powdery, dispersible sulfur, especially suitable for the purposes of crop protection - Google Patents
Process for the production of powdery, dispersible sulfur, especially suitable for the purposes of crop protectionInfo
- Publication number
- DE1024934B DE1024934B DEB38111A DEB0038111A DE1024934B DE 1024934 B DE1024934 B DE 1024934B DE B38111 A DEB38111 A DE B38111A DE B0038111 A DEB0038111 A DE B0038111A DE 1024934 B DE1024934 B DE 1024934B
- Authority
- DE
- Germany
- Prior art keywords
- sulfur
- crop protection
- dispersible sulfur
- production
- powdery
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 229910052717 sulfur Inorganic materials 0.000 title claims description 37
- 239000011593 sulfur Substances 0.000 title claims description 37
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims description 36
- 238000000034 method Methods 0.000 title claims description 11
- 238000004519 manufacturing process Methods 0.000 title claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 238000000227 grinding Methods 0.000 claims description 10
- 239000000080 wetting agent Substances 0.000 claims description 3
- 239000011814 protection agent Substances 0.000 claims description 2
- 238000003889 chemical engineering Methods 0.000 claims 1
- 239000000047 product Substances 0.000 description 6
- 239000000243 solution Substances 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 239000000084 colloidal system Substances 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 210000000056 organ Anatomy 0.000 description 2
- 239000005077 polysulfide Substances 0.000 description 2
- 229920001021 polysulfide Polymers 0.000 description 2
- 150000008117 polysulfides Polymers 0.000 description 2
- 238000009987 spinning Methods 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 1
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 description 1
- 241000416162 Astragalus gummifer Species 0.000 description 1
- 239000004606 Fillers/Extenders Substances 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 235000009001 Quillaja saponaria Nutrition 0.000 description 1
- 241001454523 Quillaja saponaria Species 0.000 description 1
- 229920001615 Tragacanth Polymers 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 235000012538 ammonium bicarbonate Nutrition 0.000 description 1
- 239000001099 ammonium carbonate Substances 0.000 description 1
- UYJXRRSPUVSSMN-UHFFFAOYSA-P ammonium sulfide Chemical compound [NH4+].[NH4+].[S-2] UYJXRRSPUVSSMN-UHFFFAOYSA-P 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 235000013490 limbo Nutrition 0.000 description 1
- 235000014666 liquid concentrate Nutrition 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 239000008267 milk Substances 0.000 description 1
- 210000004080 milk Anatomy 0.000 description 1
- 235000013336 milk Nutrition 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000020477 pH reduction Effects 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 150000003463 sulfur Chemical class 0.000 description 1
- 150000003464 sulfur compounds Chemical class 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 230000009974 thixotropic effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/02—Preparation of sulfur; Purification
- C01B17/10—Finely divided sulfur, e.g. sublimed sulfur, flowers of sulfur
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/02—Preparation of sulfur; Purification
- C01B17/06—Preparation of sulfur; Purification from non-gaseous sulfides or materials containing such sulfides, e.g. ores
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Description
Verfahren zur Herstellung von pulverförmigem, dispergierbarem, insbesondere für Zwecke des Pflanzenschutzes geeignetem Schwefel Es ist bekannt, für die Erzeugung von pulverförinigem, beispielsweise als Pflanzenschutzmittel verwendbarem, in Wasser dispergierbarem Schwefel geeignete Schwefelverbindungen in wäßriger Lösung zu zersetzen und den dabei abgeschiedenen Schwefel durch Absitzenlassen, Filtrieren, Schleudern u. dgl. von der wäßrigen Phase zu trennen und anschließend zu trocknen. Dabei werden dem Schwefel vor der Trocknung gegebenenfalls Zusätze, wie Dispergier-und Netzmittel, Streckmittel u. dgl., beigemischt. Der so gewonnene Schwefel wird schließlich in Vorrichtungen, wie Kugel-, Stift-, Schlagkreuz- oder Strahlmühlen, zu Pulver vermahlen.Process for the production of powdery, dispersible, in particular Sulfur suitable for crop protection purposes is known for the production of powdery ones, for example those that can be used as crop protection agents, in water dispersible sulfur to decompose suitable sulfur compounds in aqueous solution and the sulfur deposited in the process by allowing it to settle, filtering, spinning and the like to be separated from the aqueous phase and then dried. Be there the sulfur before drying, if necessary, additives, such as dispersants and wetting agents, Extenders and the like, mixed in. The sulfur obtained in this way is ultimately used in Devices such as ball, pin, cross beater or jet mills are ground to powder.
Diese Arbeitsweise hat den Nachteil, daß sich der Schwefel in manchen Mühlen schon nach kurzer Zeit an den Mahlorganen festsetzt und schmilzt, wodurch der Zufluß weiteren Mahlgutes gehemmt wird und der Betrieb der Mühle unterbrochen werden muß.This procedure has the disadvantage that the sulfur in some Mills stuck to the grinding organs after a short time and melts, causing the inflow of further ground material is inhibited and the operation of the mill is interrupted must become.
Es wurde gefunden, daß man diese Nachteile vermeiden kann, wenn man den gewonnenen dispergierbaren Schwefel mit einem Wassergehalt von etwa 2 bis 20%, vorzugsweise 5 bis 15%, vermahlt.It has been found that these disadvantages can be avoided if one the obtained dispersible sulfur with a water content of about 2 to 20%, preferably 5 to 15%, ground.
Die obere Grenze des in dem Schwefel vor der Verinahlung zu belassenden Feuchtigkeitsgehaltes von etwa 20% ist durch die in diesem Bereich auftretenden Thixotropieerscheinungen des Schwefels bedingt.The upper limit of what can be left in the sulfur prior to mixing Moisture content of about 20% is due to that occurring in this area Thixotropic phenomena of sulfur conditional.
Bei der Bemessung des Wassergehaltes, mit dem der Schwefel zur Vermahlung kommt, ist zu berücksichtigen, daß das Gut beim Mahlen trockener wird. Vorteilhaft geht man von einem möglichst nassen Schwefel aus. Man verkürzt und vereinfacht dadurch auch die der Mahlung vorausgehenden Arbeitsgänge, wie Filtrieren, Schleudern usw., und vermeidet um so sicherer jegliches Verschmieren der Mühle. Anderseits bestimmen Feuchtigkeitsgrad, Feinheit und Dispergierbarkeit des gewünschten Enderzeugnisses den Wassergehalt des Ausgangsproduktes. Diese Eigenschaften des Enderzeugnisses können, wenn sie nach einmaliger erfindungsgemäßer Behandlung des Schwefels noch nicht befriedigen, durch Wiederholung der Mahlung auf die gewünschten Werte gebracht wer den.When measuring the water content with which the sulfur is used for grinding it must be taken into account that the material becomes drier when it is ground. Advantageous one assumes that the sulfur is as wet as possible. It shortens and simplifies also the operations preceding grinding, such as filtering, spinning, etc., and all the more reliably avoids any smearing of the mill. Determine on the other hand Degree of moisture, fineness and dispersibility of the desired end product the water content of the starting product. These properties of the final product can if they still after a single inventive treatment of the sulfur not satisfactory, brought to the desired values by repeating the grinding will.
Man kann nach dem vorliegenden Verfahren Schwefel behandeln, der in beliebiger Weise, z. B. aus Polysulfidlösungen durch Verkochen, Ansäuern oder Zersetzen mit Gasen, hergestellt ist.You can treat sulfur in the present process, which is in any way, e.g. B. from polysulfide solutions by boiling, acidification or decomposition with gases.
Dem Schwefel können vor der Mahlung in an sich bekannter Weise Streck-, Dispergier-, Netzmittel od. dgl. und/oder andere Pflanzenschutzmittel zugesetzt «-erden.The sulfur can be stretched in a known manner before grinding, Dispersants, wetting agents or the like and / or other pesticides added "-earth.
In den nachfolgenden Beispielen ist die Schwebezahl des Schwefels nach der im »1\Tachrichtenblatt der Biologischen Zentralanstalt«, Braunschweig, 1, S. 107 (19-19), beschriebenen Methode bestimmt. Beispiel 1 Eine bei der Regenerierung von mit Schwefel beladener Aktivkohle mit Ammoniumsulfidlösung erhaltene Ammoniumpolysulfidlösung wird in Gegenwart eines Schutzkolloids verkocht; die entstandene etwa 20%ige Schwefelmilch wird geschleudert und der dabei abgeschiedene dispergierbare Schwefel auf einen Wassergehalt von 0,2% getrocknet. Das so erhaltene Präparat,wird in einer Stiftmühle vermahlen. Schon nach kurzer Zeit treten Störungen der Mahlorgane durch Verschmieren der Stifte und Mahlscheiben mit geschmolzenem Schwefel auf. Die Schwebezahl des erhaltenen Produktes beträgt 69,3.In the examples below is the limbo number of the sulfur according to the "1 \ Tachrichtenblatt der Biologische Zentralanstalt", Braunschweig, 1, p. 107 (19-19), described method. Example 1 One in regeneration ammonium polysulfide solution obtained from sulfur-laden activated carbon with ammonium sulfide solution is boiled in the presence of a protective colloid; the resulting 20% sulfur milk is centrifuged and the dispersible sulfur separated out on one Dry water content of 0.2%. The preparation thus obtained is in a pin mill grind. Already after a short time there are disturbances of the grinding organs due to smearing the pins and grinding disks with molten sulfur on it. The floating number of the obtained product is 69.3.
Wird aber der Schwefel unmittelbar nach dem Abschleudern mit einem Wassergehalt von 16,3% auf der gleichen Mühle gemahlen, so werden keine Ansätze in der Mühle beobachtet, und es wird ein Produkt mit der Schwebezahl 59,2 und einem Wassergehalt von 9,0% erhalten.But if the sulfur immediately after being thrown off with a Water content of 16.3% is ground on the same mill, so no batches are made observed in the mill, and it becomes a product with the floating number 59.2 and one Obtained water content of 9.0%.
Nach einem zweiten Mahlgang hat das erhaltene Produkt bei einem Wassergehalt von 1,2% die Schwebezahl 65,7.After a second grinding cycle, the product obtained has a water content of 1.2% the suspension number is 65.7.
Beispiel 2 Nach dem Beispiel 1 hergestellter Schwefel wird auf einen Wassergehalt von 5,0% gebracht. Die Malilung dieses Schwefels in der im Beispiel l verwendeten Mühle verläuft störungsfrei und führt zu einem Produkt mit der Schwebezahl 70,3 und einem Wassergehalt von 0,2%.Example 2 Sulfur prepared according to Example 1 is applied to a Brought water content of 5.0%. The malilung of this sulfur in the example The mill used runs smoothly and leads to a product with the floating number 70.3 and a water content of 0.2%.
Beispiel 3 100 Gewichtsteilen des nach dem Beispiel 1 hergestellten Schwefels mit etwa 16% Wasser werden je 2 Gewichtsteile Ton und ligninsulfosaures Natrium sowie 1 Gewichtsteil Ammoniumbicarbonat zugesetzt. Das Gemisch wird in der im Beispiel 1 beschriebenen Weise gemahlen. Man erhält ein Produkt mit der Schwebezahl 65.2 und einem Wassergehalt von 5,3 %.Example 3 100 parts by weight of that prepared according to Example 1 Sulfur with about 16% water becomes 2 parts by weight of clay and ligninsulfosaures Sodium and 1 part by weight of ammonium bicarbonate were added. The mixture is in the milled in the manner described in Example 1. A product with the floating number is obtained 65.2 and a water content of 5.3%.
Das Vermahlen von Schwefel mit einem Kolloid (Leim, Tragantgummi, Seifenrindenextrakt usw.) und der erforderlichen Menge Wasser zwecks Herstellung kolloidaler Lösungen von Schwefel ist bereits bekannt. In der Patentliteratur ist die Herstellung von feinverteiltem Schwefel als flüssigem Konzentrat beschrieben, wobei von kristallinem Schwefel ausgegangen wird, der mit Wasser zu einem dicken Schlamm mit einem Schwefelgehalt von bis höchstens 72% angerührt wird, und wobei die Zerkleinerung des Schwefels in Scheibenmühlen erfolgt und das dabei erhaltene Endprodukt normalerweise nur etwa 28% Schwefel enthält.The grinding of sulfur with a colloid (glue, gum tragacanth, Soap bark extract, etc.) and the required amount of water for production colloidal solutions of sulfur is already known. In the patent literature describes the production of finely divided sulfur as a liquid concentrate, where crystalline sulfur is assumed, which becomes thick with water Sludge with a sulfur content of up to a maximum of 72% is mixed, and where the sulfur is crushed in disk mills and the resulting Final product usually only contains around 28% sulfur.
Während diese Verfahren zum Ziel haben, einen dispergierbaren Schwefel aus nicht dispergierbarem Schwefel herzustellen, geht man beim vorliegenden Verfahren von einem in beliebiger Weise hergestellten, bereits dispergierbaren Schwefel aus und führt diesen dispergierbaren Schwefel in pulverige Form über.While these methods aim to provide a dispersible sulfur Preparing from non-dispersible sulfur is an acceptable approach in the present process from an already dispersible sulfur produced in any way and converts this dispersible sulfur into powdery form.
Claims (3)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DEB38111A DE1024934B (en) | 1955-12-01 | 1955-12-01 | Process for the production of powdery, dispersible sulfur, especially suitable for the purposes of crop protection |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DEB38111A DE1024934B (en) | 1955-12-01 | 1955-12-01 | Process for the production of powdery, dispersible sulfur, especially suitable for the purposes of crop protection |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| DE1024934B true DE1024934B (en) | 1958-02-27 |
Family
ID=6965398
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DEB38111A Pending DE1024934B (en) | 1955-12-01 | 1955-12-01 | Process for the production of powdery, dispersible sulfur, especially suitable for the purposes of crop protection |
Country Status (1)
| Country | Link |
|---|---|
| DE (1) | DE1024934B (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2604695A1 (en) * | 1975-09-15 | 1977-03-24 | Pasq Mormino & Figlio Termini | Water-dispersible anti-cryptogamic sulphur paste - contg. e.g. sulphur, calcium lignin sulphite, disinfectant, protective colloid and water |
| WO1990003350A1 (en) | 1988-09-30 | 1990-04-05 | F.P.S. Italiana - Finances Products Services S.R.L. | Sulfur-based chemical soil-corrective in the form of pellets for agricultural use |
| WO2008084495A3 (en) * | 2007-01-08 | 2008-10-02 | Deepak Pranjivandas Shah | Novel agricultural composition |
| US8814976B2 (en) | 2009-04-16 | 2014-08-26 | Sulvaris Inc. | Dispersible sulphur fertilizer pellets |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE290610C (en) * | ||||
| US2658016A (en) * | 1948-08-31 | 1953-11-03 | Brown Laurie Oakley | Production of fine aqueous dispersion of sulfur |
-
1955
- 1955-12-01 DE DEB38111A patent/DE1024934B/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE290610C (en) * | ||||
| US2658016A (en) * | 1948-08-31 | 1953-11-03 | Brown Laurie Oakley | Production of fine aqueous dispersion of sulfur |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2604695A1 (en) * | 1975-09-15 | 1977-03-24 | Pasq Mormino & Figlio Termini | Water-dispersible anti-cryptogamic sulphur paste - contg. e.g. sulphur, calcium lignin sulphite, disinfectant, protective colloid and water |
| WO1990003350A1 (en) | 1988-09-30 | 1990-04-05 | F.P.S. Italiana - Finances Products Services S.R.L. | Sulfur-based chemical soil-corrective in the form of pellets for agricultural use |
| WO2008084495A3 (en) * | 2007-01-08 | 2008-10-02 | Deepak Pranjivandas Shah | Novel agricultural composition |
| CN101657395A (en) * | 2007-01-08 | 2010-02-24 | 迪帕克·普兰吉万达斯·沙阿 | Novel agricultural composition |
| US8241387B2 (en) | 2007-01-08 | 2012-08-14 | Deepak Pranjivandas Shah | Agricultural composition |
| CN101657395B (en) * | 2007-01-08 | 2014-03-12 | 迪帕克·普兰吉万达斯·沙阿 | Agricultural composition |
| US8814976B2 (en) | 2009-04-16 | 2014-08-26 | Sulvaris Inc. | Dispersible sulphur fertilizer pellets |
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