DE1900781A1 - Process for the preparation of mixtures of sodium tripolyphosphate and a silicate in the form of strong, stable particles - Google Patents

Description

DR. ELISABETH JUNG, DR. VOLKER VOSSlUS, DIPL.-ING. GERHARD COLDEWEY

MÖNCHEN 23 SIEGESSTRASSE 26 TELEFON 34 SO 67. TE L E G R AM M-AD R ES S E: INVENT / MÜNCHEN

B-Jan, Ι3Ξ9

D 9o3 (La / Vo / Rti)
PMO

FMG CORPCR.1ΪΙ0Μ
New York, NY, V.St.A.

Process for the preparation of mixtures of sodium tripolyphosphate and a silicate in the form of strong, stable particles

Priority: January 8, 1968, V.St.Ä., No. ₉ 696

The invention relates to the production of strong, stable particles which are a mixture of a polyphosphate and a silicate and should serve as a cleaning agent

For the production of a cleaning agent present as a dry mixture, the 2.B. Use as a dishwashing detergent
is to find, sodium tryphosphate is generally used as the basic substance together with other conventional additives. Such substances can be anionic or non-ionic synthetic surface-active compounds, precipitated

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preventive substances such as sodium arboxymebhy! cellulose, Sbi'eükriitt-.slj DuftsfcoC-fe, bleach, such as chlorinated qranurates, or alkaline agents. like sodium carbonate and KatriumhydroxycV The so-called, based on polyphosphate alkaline detergents are known for -that them when used in both normal dishwashers and washing machines on metals as well as on enamel goods with which they are in Come into contact, have a corrosive effect. To now such a Avoid corrosion in such detergents Älkal.i.aatailail lltat «, mostly sodium silicate, incorporated.

When such mixtures are made from catalytic tripolyphosphate; and one in silicate in dry-mixed cleaning races often cause problems. The components bake together into hard agglomerates which are difficult to pour and handle and which also cause undesired excretion of individual components. A method for preventing the undesired caking of such masses is described in the USA patent specification NT, 2 $ 09 49o. Here it is described how such a two-component mixture of sodium tripolyphosphafe and sodium silicate can be produced by using the components mixes at temperatures below 60 °, the anhydrous sodium tripolyphosphate dehydrating the VässPi £ -liquid sodium 11 ikafc.untep formation of a troclcenei: mixture dehydrated,.-..-. ^_-:::; '^ ;;> - ,, ■ ·'": - -. ■.-.-:

Piases two-component geniisph shows, however, certain evidence

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190Q781

Share on «First of all, it can only be produced using weakly Altolian silicates, eg those silicates, which have a weight ratio SiOgIKa ₂ O of 3» 22: 1 bit 2, * to: 1 * Furthermore, if a high molar proportion of silicate opposite polyphosphate is desired _f z, B _e MoI a ratio of at least 1: 1 to achieve, "an optimal corrosion prevention ,, one can only weakly alkaline silicate (Gewiehtsverhältnis SiOgtüa ^ O of 3.22: 1) using _{f to} get the Zvreikowponenten ~ product ,, This is a nacj · part. * "Eil strongly alkaline components for producing sol" rather cleaner slsdr particularly desirable such, in l <"strength i # ssriger ϊ & βχαακ a _pH value of at least Ιο, ί aaftfßisen to achieve, inter alia, both better Reiniocungswirkung, and the To avoid the occurrence of precipitations in the solutions of such detergents »

Buttocks YOsflie ^ BBäer EpfindüBf vsserde "Semische aus Natriuntri" polyphoshphat and eiaerp SIl! test to Pcarra stronger, more stable ^ particle selects a "volume ratio of silicate to sodium trl"

vo & ffiindestens i: condition 1, in l # -ißer solution p ^ value iron of at least Iq, 5 to have ,, prepared by iaan a wässriRe solution of a NatriuwstliTcats that a weight ratio SiOgINa ₂ O of less than 2, * to : l has to a Schüttuns? from pulverized, water-bituminous phosphate solaa ^ each added until the molar ratio SiO ₂ to tripolyphosphate is at least 1: 1, and a moist mixture of these components is formed

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nian this wet mixture is stirred until _f deformable plastic grains / ?, 'earth? i _r this Diastischen.Körner in a heating zone at temperature s of about 6o ° to 8 ο ⁰ C ss * ltit ^ ₈ to the graininess? "fcj'oe-cen: -:}. ncL and then grinds and seventh

When carrying out the present invention, use is made of: i? 2; erui \ '! 3rte.o, inter alia, triun tr! Poly phosphate, If the sodium tripoly-phosphate is not in powdered form, it has to be used according to''3VjT:. .o] ri-ii method milled until the poly phosphate in Aichnn we sent-τ in sieve with o _s j3 now clear mesh width and wfenig- to about 3 <> ^c "~ a sieve to au o _f 175 mm internal mesh pasöiei't, »Then the sodium tripolyphosphate is converted into a k, zR a ribbon mixer or a mixing drum *

The sodium silicate should have a weight ratio SiO ₂ : Wa ₂ O below 2.00: 1. Particularly useful «» Hodium silicate solutions are those from the Philadelphia Quartz Company, as listed below:

Name Wt .- ^ Well _? 0 wt .- ^ SiO _? Wt .- ^ H ₉ O wt. Ratio

of the product * S10 «: Na _o 0

D. 14th »7 29 Λ C. 18th "O 36 .0 B-W 19th .5 31 .2

55. 9 2 .oo: l 46. O 2 .οο.Ί 49. 3 1 .8o: l

The Silikatlösunnc is then converted into the Na tr tr ium phosphate iwoly "IISS · using fuel nozzles or other distribution means 909837/1380

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wv :, it is continuously entered and dispersed, Ms : 1ns molar ratio of SiO ₉ to tripolyphosphate at least.)>: 1. The mixture becomes damp and clumps to form hfsio ^! 'on, plastic and deformable grains together. The grains were then heated in a heating chamber to 60 ° to 80 ° C., in the course of which they lost moisture. In this Tempsi-afcur the grains are left as long as they are dry to, they will, if necessary, p; _r emahlen so that they in wesQ-itlicher) a sieve of at most 2.36 to at least o, 29 "ran lights Masehsnweite happen. Fractions with a mesh size of less than 0.29 g are moved out into the reaction chamber and mixed with further ground polyphosphate before further siliceous solution is added.

A sodium silicate solution like the one mentioned above, which contains about 55% of water, can be used as it is obtained from the manufacturer and added directly to the sodium tripolyphosphate. Sometimes, however, it is desirable to add enough water (max. Io %) to the silicate solution until the water level is reached; the solution reaches about 60 wt. which do not have the iced degree of stickiness to achieve soft, plastic and malleable grains. The formation of these deformable grains is

^Λ ο

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VH1.T "DuvehfOhruttg of the present invention is necessary because ·· r> i5.fc mar; mt? H rJ.i / n drying obtains strong grains which have an eroded density n.ledore, e.g.« from about 0.7 to about 0.8 κ / οπτ 2, vfwe? 3on, and dia do not crumble if you mix them in dry « \ o / i) nm " ».stand tnifc other 'additives in a mixer *

■ / iolc'Aoh isb as' iwoekmäsjsig, the sodium silicate solution klsi- ! • ißjff: fen ^ Gii a Hetsmittel, e.gn a Oberfläschetiaktivts MihfcoL, EuzusebKen, around a ^ leichmässijie wetting of the wasnerfrejan Haferium tripolyphoaphats and at the same time o.in a uniform mixture with shortened mixing time to certain mr.e-p, Suitable wetting agents are lower universal ethers of oxy-phenyl-alcoholic acid adducts, like those under the trade

i Triton CP available products "eg Triton CP-54, -i ¹ -Rutylether of an octylphenol-ethylene oxide adduct, and Aton X * loo, oin itoctylphenol-ethylene oxide adduct"

For convenience, the mixing process is done at room temperature carried out but higher temperatures can also! may be used, provided that there are no major Lots of water to be evaporated.

In the production of the product according to the invention, it is as already said above, desired the ratio of

to sodium tripolyphosphate at least at 1; 1, z "/ ar ₄ to achieve good corrosion prevention"

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γ ;;. ιϊ .'S'.jlohGn ratio of Siliitat to I3a tr iumtripoly phosphate ranges Auss _f to a corrosion of the metallic material by illustrates erfindunscsgeniässe detergent in to avoid completely or substantially. Smaller amounts of silicates are not so! «/ Ineffective»

The examples illustrate the invention.

example 1

11.3 ^ 4- kg powdered sodium tripolyphosphate with the following Grain size distribution:

4.9 % o, 38 - o _s 29 mm clear mesh size

9.1 <f » o _f 29 - o _t 2o mm clear mesh size

12, ο 35 o _f 2o-o, 15 mm clear mesh size

74 _r o i> below 0.15 mm clear mesh world

and having a bulk density of from o, 93 g / cnr to be "placed in a rotor mixer, the mixer has a Durohmesser of 45 _r 7 cm and a length of 45.7 cm and contains seven 5 cm high thread _f change the contents to circulate . The mixer wire, then switched on and set to a speed of 15 per minute. While the mixer rotates, letting a mixture of 7.8 kg silicate solution (product of "Philidelphia Quartz Company", containing 14.7% Na ₃ O, 29.4 <SiO ₂ and 55.9 ^ HgO) and o _r 23 kg water (Iqulvalent 3 weight 5ß water to reduce the viscosity of the. silicate solution) with a l _t 3 cm in diameter einfliesfc'en measuring pipe in the mixer, the end of the tube, which is located in the mixer containing 8 Small openings about 5 cm apart

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which vilrd the silicate solution finely distributed in the circulated embankment of sodium tri-poly phosphate. The entire silicate solution is added in the course of 20 minutes. The sherge becomes damp and the powdered material clumps together to form irregular lumps that become sticky and plastic. These plastic lumps are dried at 65 ° C until they are hard, then they are ground and sieved * About 80 % of the ground particles are separated as a granular product which has a particle size between 2.4

"and o _{f has} a mesh size of 3 mm with a volume density of O ₄ 85 g / ml, while about 20 f 'has a particle size of less than 3 mm open mesh size. A sample of the granular product is dissolved in a 1 ß aqueous solution which is completely free from insoluble matter and has a p "" value of lo,.? having. The granular product contains 19.5 # total moisture (loss on ignition) and has a molar ratio of SiOg to sodium tripolyphosphate of 1.23: 1. To determine the firmness of the granular product,

r a sample of it with other common cleaning agents in mixed with a mechanical stirrer, whereby neither the granular structure of the product is lost nor an increase in the Bulk density is determined.

Example 2

The procedure of Example 1 is repeated with the difference that only 9, o? kg of powdered sodium tripolyphosphate together with 2 _t 2? kg of the according to example 1

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obtained granular product with a grain size below O ₇ ?.? there is a clearer distance. Farner the amount dei added Silikatlösimg is reduced by 2o% "The speed 'lan addition of the silicate solution is reduced and erΐordert now accounts for 36 minutes The resulting sticky Klumpan be as long as likewise dried at 65 ° C until aind, and then gcroahlon and sifted., about 80 "i des

n approach are as a granular product with a grain size between 2.4 mm and 0.29 n in the clear mesh size with a bulk density of o _? 76 g / ciir gained. A sample of the obtained product is dissolved to a 1 ^ aqueous solution containing no insoluble components and having a p "value of lo.7, The product contains 2o, 5 ^ Total ·« moisture (loss on ignition) and has a Molar ratio of SiOp to sodium tripolyphosphate of 1.23: 1. The product consists of hard grains that do not break when mixed mechanically with other detergents.

Example 3

The procedure according to 'Example 1 is repeated with the difference, 13.6 kg of powdered sodium tripolyphosphate with the following particle size distribution are obtained:

0.9 *> o _t 29 - o.25 mm clear mesh size

2.1 K> 0.25 - 0.22 mm clear mesh size

8.8 £ o, 2o-o, 15 mm clear washing width

88.2 H below 0.15 mm clear masonry width

and used with a bulk density of o.91 g / cm ^J. A

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.? Iron Natriumtrinolyphoaohat in the course of an hour, with stirring added The Iialrtumsilikatlösung will not go; ■> epi i5oh of 8.6 kg of the sodium silicate solution and 0.35 kg Triton ".Vi.oo (N-stznlttel) ui ^r like a Schüttnnq. of water are added Di3 resulting sticky and plastic lumps are then ccetrocknst at 6'3 ° C, ground and screened about 8o i> of e * -... approach preserved have a particle size between 2.36 nm and o, 2Q ram lights Masehenweite. the bulk density beträft o, 68 g / cm, daa Molvorhältnis of SiO ₂ to 1.22 sodium tripolyphosphate. 1 and the total moisture (loss on ignition) 19.9 ¹ 'a sample d63 granular product is in a 1 YSS-ig wäßs ^ i / In this example the slow addition of the silicate solution and the use of a wetting agent apparently reduce the bulk density of the process product.

example k

9.07 kg of powdered sodium tripolyphosphate with a particle size distribution as in example 3 are placed at 75 ° C. in a heater as in example 1; 2.27 kg of the product from Example 3 with a grain size of _{less than o t} 29 mm clear width are added. A mixture of 5.72 kg of the silicate solution used in Example 1, 0.18 kf; Water and 0.24 kg of Tergitol Min-Poaia (Hetzmittel from "Union Carbide Co.", a modified adduct of an unbranched alcohol and ethylene oxide) is added over the course of 27 minutes

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g of sodium tripojlyphosphate given. The mixture consists almost entirely of a pi- "-! - 1'1CT moist wetness of a grain size between ty.7o mm iii"; ^: ... mm clear I ^ ashr-in width. The product will continue to be available for as long as 65 ^f ■., -Etroo ^ iVit. "until it is hard _r then it is ground and" μ ";·; * ·; po _r . '^" boretrer-nth larger portion of the product has a liorn size ö ^ vsrtailung between 2 _; 36 κιπι and ο _£ 29 now open throat width, with a bulk density \ τ _Ο η ο, 79 g / cnr, an "isaamtfeuchtipckeit of 16.6 # (loss on ignition) and a;! .-] - '. "iltnis, lo of sodium tripolyphosphate to SiOg of l:..! l _L ^ i.nc · oue ■ the product obtained is dissolved in a 1 # wäserSfren strength solution containing a p" value of ~ lo _t 6 has, The dry product consists of hard grains that do not break or dust when washed with other cleaning agents in a mechanical agitator.

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Claims (1)

1, A process for the preparation of mixtures of Natriumtripoly-phosphate and a silicate in the form of strong, stable particles having a Holverhältnis of silicate to sodium tripolyphosphate of at least 1: 1, the lo in 1 £ -lger aqueous solution has a p _H ~ value of at least, 5, characterized in that an aqueous solution of sodium silicate, which has a weight ratio of SiO ₂ : Na ₂ O of below 2.4o: 1, is made up of a bed powdered sodium polyphosphate is added until the molar ratio of SiO ₂ to tripolyphosphate is at least 1: 1 and a moist mixture of these components is obtained, so that the moist mixture is then stirred, bit: deformable plastic grains are obtained, these plastic grains in heated in a heating zone to temperatures of about 6o ° C to 8o ° C until the grains are dry, and then grinds and sifts. 2. The method according to claim 1, characterized in that an aqueous solution of a sodium silicate may be used, which has a weight ratio SlO ₂ : Na ₃ O of 2.0: 1. 3. The method according to claim 1 and 2, characterized in that an aqueous solution of a sodium silicate is used which contains a wetting agent. 909837/1380 "The method of claim I ₁ characterized in that powdered Natriuratripolyphosphat used, the In" / es ent borrowed a sieve 0.38 mn old lights washing space and at least about 5O a sieve of up to o _f 175 mm happens liohter mesh " "Process according to claim 1, characterized in that up to particles of a mesh size between 2.36 ram, the sieving of the ground Verfahrensprcduktes and performs O ₃ 29 pun liohter Maseheiroeite. 909837/1380