DK163225B - PROCEDURE FOR CONTINUOUS PREPARATION OF SODIUM PERBORATE MONO HYDRATE FROM THE TETRA HYDRATE - Google Patents

PROCEDURE FOR CONTINUOUS PREPARATION OF SODIUM PERBORATE MONO HYDRATE FROM THE TETRA HYDRATE Download PDF

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DK163225B
DK163225B DK086386A DK86386A DK163225B DK 163225 B DK163225 B DK 163225B DK 086386 A DK086386 A DK 086386A DK 86386 A DK86386 A DK 86386A DK 163225 B DK163225 B DK 163225B
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sodium perborate
air
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fluidization
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Jacques Dugua
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Atochem
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B15/00Peroxides; Peroxyhydrates; Peroxyacids or salts thereof; Superoxides; Ozonides
    • C01B15/055Peroxyhydrates; Peroxyacids or salts thereof
    • C01B15/12Peroxyhydrates; Peroxyacids or salts thereof containing boron
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B15/00Peroxides; Peroxyhydrates; Peroxyacids or salts thereof; Superoxides; Ozonides
    • C01B15/055Peroxyhydrates; Peroxyacids or salts thereof
    • C01B15/12Peroxyhydrates; Peroxyacids or salts thereof containing boron
    • C01B15/126Dehydration of solid hydrated peroxyborates to less hydrated or anhydrous products

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Abstract

1. Process for continuous production of sodium perborate monohydrate by dehydration of sodium perborate tetrahydrate in only one step in a bed fluidized by means of a current of hot air, characterized in that the temperature of the air is between 100 C and 180 C when it enters the fluidization zone and that, in the said zone, the temperature is between the fusion temperature of sodium perborate tetrahydrate and 80 C and the relative humidity is below 40% and at least 10%.

Description

iin

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Den foreliggende opfindelsen angår en fremgangsmåde til kontinuert fremstilling af natriumperborat-mono-hydrat ved dehydratisering af natriumperborat-tetra-hydrat i fluidiseret leje ved hjælp af en strøm af varm 5 luft'.The present invention relates to a process for the continuous production of sodium perborate monohydrate by dehydrating sodium perborate tetrahydrate in fluidized bed by means of a stream of hot air.

Natriumperborat med bruttoformlen NaBO^Hg, betegnet som natriumperborat-tetrahydrat, anvendes i almindelighed til fremstilling af vaskemidler. Det er dog i besiddelse af karakteristika, såsom f.eks. opløsningshastigheden eller 10 temperaturstabiliteten, som stadig er utilstrækkelig til, at det giver fuld tilfredsstillelse under dette anvendelsesområde .Sodium perborate of the gross formula NaBO 3 Hg, designated as sodium perborate tetrahydrate, is generally used for the preparation of detergents. However, it possesses characteristics such as e.g. the dissolution rate or temperature stability, which is still insufficient to provide full satisfaction under this scope.

Der ud over foretrækker man mere og mere det såkaldte na-triumperborat-monohydrat med bruttoformlen NaBO^l·^, som 15 er i besiddelse af, især i forhold over for natriumper borat-tetrahydrat, et indhold af aktiv oxygen, som er ca. 50¾ større, og en hurtigere opløsningshastighed.In addition, the so-called sodium tri-boro borate monohydrate of the gross formula NaBO + l, which is in possession of, in particular with respect to sodium per borate-tetrahydrate, is more preferably an active oxygen content which is approx. 50¾ larger, and a faster resolution rate.

De hidtil kendte fremgangsmåder til fremstilling af na-triumperborat-monohydrat ud fra natriumperborat-tetra-20 hydrat består i fra dette at fjerne den ønskede mængde krystalvand ved hjælp af en strøm af varm luft.The known methods for producing sodium triborate monohydrate from sodium perborate tetrahydrate consist of removing the desired amount of crystal water by means of a stream of hot air.

For at sikre en god fordeling af den varme luft såvel som en god ensartethed af temperaturen i den masse, som skal dehydratiseres, og for at undgå en overdreven nedbrydning 25 af denne masse, har man foreslået at gennemføre dehydra- tisering af natriumperborat-tetrahydrat i fluidiseret leje ved hjælp af en strøm af varm luft.In order to ensure a good distribution of the hot air as well as a good uniformity of the temperature of the mass to be dehydrated, and to avoid excessive decomposition of this mass, it has been proposed to dehydrate sodium perborate tetrahydrate in fluidized bed using a stream of hot air.

Dette beskrives i fransk patentskrift nr. 1 081 421, i-følge hvilket teknikken med anvendelse af fluidiseret leje 2This is described in French Patent No. 1,081,421, according to which the technique of using fluidized bed 2

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gør det muligt at opretholde i den masse, der skal dehy-dratiseres, en homogen temperatur på mellem 50 °C og 60 °C.allows the mass to be dehydrated to maintain a homogeneous temperature of between 50 ° C and 60 ° C.

Det er imidlertid nødvendigt, for at opnå kontinuert under anvendelse af denne teknik med fluidiseret leje korn af 5 perborat-monohydrat, som er modstandsdygtighed over for nedslidning, at arbejde ifølge fransk patentskrift nr.However, in order to obtain continuously using this fluidized bed technique grain of 5 perborate monohydrate which is resistant to wear and tear, it is necessary to work according to French patent specification no.

2 013 104 med en strøm af luft, hvis temperatur er højere end 180 °C ved indgangen til fluidiseringszonen, eller også, dersom dette ikke er tilfældet, samtidig at svare 10 til det dobbelte krav fremsat i det franske patentskrift og i additionscertifikatet, som er offentliggjort henholdsvis under numrene 2 207 859 og 2 285 339, at man har en relativ fugtighed i den cirkulerende luft i fluidiseringszonen lig med mindst 40% og højst 80%, og at temperaturen 15 på luften, når den forlader denne zone, mindst er lig med 60 °C.2 013 104 with a flow of air whose temperature is higher than 180 ° C at the entrance to the fluidization zone, or, if not, at the same time meeting the double requirement set out in the French patent and in the addition certificate which is disclosed respectively under Nos 2 207 859 and 2 285 339 that the relative humidity of the circulating air in the fluidization zone is at least 40% and at most 80%, and that the temperature 15 of the air when leaving this zone is at least equal at 60 ° C.

En kontinuert gennemførelse af dehydratisering i fluidiseret leje ifølge den fremgangsmåde, som er beskrevet i det først ovenfor nævnte patentskrift, fører til et mono-20 hydrat, hvis kvalitet beklagelig vis er nedbrudt ved den fastslåede tilstedeværelse af en hastigt forøgende mængde af skrubber af dimensioner, som overskrider de specifikationer, som godtages af anvenderne.A continuous implementation of fluidized bed dehydration according to the method described in the aforementioned patent leads to a monohydrate whose quality is deplorably degraded by the established presence of a rapidly increasing amount of scrubber of dimensions. which exceeds the specifications accepted by the users.

De fremgangsmåder, som er beskrevet i de to øvrige doku-25 menter, medfører ikke alene i praksis mindst to hydrati-serings-trin; men de fører yderligere til dannelsen af meget fine partikler, der kan betegnes som støv, og som, når de er fraseparerede fra den strøm af fugtig luft, der betegnes som dehydratiseringsluften, og som medbringer 30 dem uden for fluidiseringszonen, behøver at blive tilbageført til natriumperborat-tetrahydrat-tilstanden, før de på ny kan indgå i dehydratiseringsprocessen.The methods described in the other two documents not only in practice entail at least two hydration steps; but they further lead to the formation of very fine particles which can be termed dust and which, when separated from the stream of moist air referred to as the dehydration air and which carry them outside the fluidization zone, need to be returned to the sodium perborate tetrahydrate state before they can be included again in the dehydration process.

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33

Fremgangsmåden ifølge den foreliggende opfindelse gør det muligt at undgå ulemperne knyttet til de kendte fremgangsmåder og kontinuert at oonå i pf enkelt trin korn af na-triumperborat-monohydrat med høj modstandsdygtighed over 5 for slid ved nedslidning, under driftsbetingelser, som ikke kunne lade formode, at det var muligt at opnå et sådant resultat.The process of the present invention makes it possible to avoid the disadvantages associated with the known processes and to continuously in pf single-step cereals of high-resistance sodium boron borate monohydrate above wear and tear, under operating conditions which could not presume, that it was possible to achieve such a result.

Fremgangsmåden består af en kontinuert fremgangsmåde til fremstilling af natriumperborat-monohydrat ved dehydrati-10 sering af natriumperborat-tetrahydrat i et enkelt trin i fluidiseret leje ved hjælp af en strøm af varm luft, og fremgangsmåden er ejendommelig derved, at luftens temperatur er på mellem 100 °C og 180 °C, når den træder ind i fluidiseringszonen, og at i denne zone temperaturen er 15 på mellem smeltetemperaturen for natriumperborat-tetrahy drat og 80 °C, og at den relative fugtighed er mindre end 40¾ og mindst lig med 10¾.The process consists of a continuous process for producing sodium perborate monohydrate by dehydrating sodium perborate tetrahydrate in a single stage in fluidized bed by a stream of hot air, and the process is peculiar in that the temperature of the air is between 100 ° C and 180 ° C when entering the fluidization zone, and in this zone the temperature is 15 between the melting temperature of sodium perborate-tetrahydric and 80 ° C, and the relative humidity is less than 40 ° and at least equal to 10 °.

Når luften ved indgangen til fluidiseringszonen har en temperatur lavere end 100 °C, er det stadig muligt at 20 arbejde inden for rammerne af de øvrige karakteristika ifølge opfindelsen; men produktiviteten bliver hurtigt meget lille, hvis man skal tilfredsstille de industrielle krav inden for dette område.When the air at the entrance to the fluidization zone has a temperature lower than 100 ° C, it is still possible to operate within the scope of the other characteristics of the invention; but productivity will quickly become very low if one is to meet the industrial requirements in this field.

Når denne temperatur når op på eller overskrider 180 °C, 25 påbegyndes dannelsen af skorper mere og mere, hvilket umiddelbart medfører de ovenfor beskrevne ulemper.As this temperature reaches or exceeds 180 ° C, crust formation begins more and more, immediately causing the disadvantages described above.

Det foretrukne temperaturområde er 130 °C - 175 °C.The preferred temperature range is 130 ° C - 175 ° C.

Det er muligt at arbejde, således som det er anført i opfindelsen; men med en temperatur i fluidiseringszonen 30 uden for det ovenfor definerede temperaturområde.It is possible to operate as stated in the invention; but with a temperature in the fluidization zone 30 outside the temperature range defined above.

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Når det drejer sig om temperaturer højere end 80 °C vil dog den ekstra tilførelse af varmeenergi, som må tages i betragtning, i praksis ikke føre til nogen mærkbar·.forbedring af det resultat, som opnås ved fremgangsmåden gen-5 nemført under karakteristika ifølge opfindelsen.However, in the case of temperatures higher than 80 ° C, the additional supply of heat energy which must be taken into account will not in practice lead to any appreciable improvement of the result obtained by the process carried out under the characteristics of invention.

Når det drejer sig om en temperatur lavere end smeltetemperaturen for natriumperborat-tetrahydrat, bliver modstandsdygtigheden over for slid ved nedslidning af det opnåede natriumperborat-monohydrat hurtigt utilstrække-10 lig.At a temperature lower than the melting temperature of sodium perborate tetrahydrate, the resistance to abrasion by wearing down the obtained sodium perborate monohydrate quickly becomes insufficient.

Luftens relative fugtighed i fluidiseringszonen er fortrinsvis på mellem 15¾ og 30¾. Opholdstiden i fluidise-ringszonen er ikke kritisk. Den kan af den grund antage meget forskellige værdier, f.eks. være på mellem 10 og 15 60 minutter idet man vælger de øvrige parametre, såsom lejets højde, fordelingen af den gasformige strøm, således, at man normalt respekterer kriterierne for fluidise-r ing.The relative humidity of the air in the fluidization zone is preferably between 15¾ and 30¾. The residence time in the fluidization zone is not critical. It can therefore assume very different values, e.g. be between 10 and 15 60 minutes, choosing the other parameters, such as the height of the bed, the distribution of the gaseous flow, so as to normally respect the criteria for fluidization.

Fremgangsmåden ifølge opfindelsen kan gennemføres i et 20 vilkårligt apparat, som almindeligvis anvendes til flui- disering af gas og fast stof, og som er konstrueret af et materiale, som er modstandsdygtigt over for korrosion ved hjælp af fugtig luft og over for nedslidning grundet bevægelsen af faste stoffer, såsom f.eks. glas eller, hyp-25 pigst, rustfrit stål.The process according to the invention can be carried out in any apparatus commonly used for fluid and gas fluids, and which is constructed of a material which is resistant to corrosion by humid air and to wear due to the movement of solids such as e.g. glass or, hypiglyst, stainless steel.

Apparaturet består i hovedsagen af en cylindrisk fluidi-serings-reaktor, som er i besiddelse af et fordelings-system for den i bunden indførte luftmængde, som er mest mulig homogen inden for fluidiseringsmassen, et system 30 til bortfjernelse af dehydratiserings-luften anbragt på toppen af reaktoren oven over den fluidiserede masse, et system til indførsel af det perborat, der skal dehydrati-seres, og som ligeledes befinder sig i den øvre del afThe apparatus consists essentially of a cylindrical fluidization reactor which has a distribution system for the bottom introduced airflow which is as homogeneous as possible within the fluidization mass, a system 30 for removing the dehydration air located on the top. of the reactor above the fluidized mass, a system for introducing the perborate to be dehydrated and also located in the upper part of the

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5 reaktoren, et udtag for natriumperborat-monohydrat ved overflydning til det ydre af den fluidiserede masse, såvel som af et system, som gør det muligt effektivt at isolere de korn, som medrives uden for fluidiseringszo-5 nen af dehydratiserings-luften, og som i almindelighed består af en eller flere cykloner.5, the reactor, an outlet for sodium perborate monohydrate, by overflowing to the exterior of the fluidized mass, as well as by a system which effectively isolates the grains entrained outside the fluidization zone of the dehydration air and which generally consists of one or more cyclones.

De således isolerede korn, som sædvanligvis ville skulle føres tilbage til tetrahydrat-tilstanden, før de kunne recirkuleres under denne form og på ny blive dehydrati-10 set, lader sig ved fremgangsmåden ifølge opfindelsen an vende direkte som bestanddele i det fremstillede natrium-perborat-monohydrat, når mængden deraf ikke overskrider ca. 10 vægt-% af vægten af det dannede natriumperborat-monohydrat.The grains thus isolated, which would usually have to be returned to the tetrahydrate state before they could be recycled under this form and again dehydrated, can be used directly in the process according to the invention as constituents of the sodium perborate produced. monohydrate when the amount thereof does not exceed approx. 10% by weight of the sodium perborate monohydrate formed.

15 Denne yderligere fordel opnås i almindelighed i praksis ved behandlingen af industriel natriumperborat-tetrahy-drat, når den opad stigende lineære hastighed af den gasstrøm, som bevæger sig igennem fluidiseringszonen, målt under de betingelser, som hersker ved udgangen fra denne 20 zone, ikke overstiger ca. 0,5 m/s.This additional advantage is generally obtained in practice in the treatment of industrial sodium perborate tetrahydrate when the upwardly increasing linear velocity of the gas flow passing through the fluidization zone, measured under the conditions prevailing at the exit from this zone, is not exceeds approx. 0.5 m / s.

De efterfølgende eksempler belyser fremgangsmåden ifølge opfindelsen.The following examples illustrate the process of the invention.

De værdier, som er angivet for den lineære opad stigende hastighed af den gasstrøm, som bevæger sig igennem flui-25 diseringszonen, er målt under de betingelser, som hersker ved udgangen fra denne zone.The values given for the linear upward velocity of the gas flow moving through the fluidization zone are measured under the conditions prevailing at the exit from this zone.

I hver af eksemplerne var det vægtmæssige udbytte mindst 99¾ under hensyntagen til det perborat, som er medrevet med dehydratiserings-luften, og som er isoleret ved cy-30 klonbehandling af denne luft og i hvert tilfælde direkte anvendt som bestanddel af det fremstillede produkt.In each of the examples, the weight yield was at least 99¾, taking into account the perborate entrained with the dehydrating air, which is isolated by cyclone treatment of this air and in each case directly used as a component of the product produced.

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De værdier, som er anført under udtrykket nedslidnings-grad, er blevet bestemt på følgende måde: man underkaster i 6 minutter 50 g af perboratet indvirkning af 8 kugler af rustfrit stål med 20 mm diameter indeholdt i en hori-5 sontal cylinder af rustfrit stål med indre diameter 100 mm og med en længde på 115 mm, som drejer sig med en hastighed på 150 omdrejning/minut. Nedslidningsgraden bedømmes således som værende den vægt-% del af perboratet, som har en kornstørrelse mindre end 53y.um.The values given under the term wear rate have been determined as follows: For 6 minutes, 50 g of the perborate effect of 8 stainless steel balls of 20 mm diameter contained in a stainless steel horizontal cylinder is subjected with an internal diameter of 100 mm and a length of 115 mm, which rotates at a speed of 150 rpm. Thus, the degree of attrition is judged to be the weight percent of the perborate having a grain size less than 53 µm.

10 Målingerne af de specifikke overflader af det fremstil lede produkt gennemføres i overensstemmelse med den såkaldte BET-metode.The measurements of the specific surfaces of the manufactured product are carried out in accordance with the so-called BET method.

Den tilsyneladende densitet af det fremstillede natrium-perborat-monohydrat var større end 0,5 g/ml.The apparent density of the sodium perborate monohydrate produced was greater than 0.5 g / ml.

15 EKSEMPEL 1EXAMPLE 1

Man anbringer i en fluidiseringsreaktor, som i hovedsagen består af et cylindrisk rør af rustfrit stål med diameteren 90 mm, 0,3 kg/h natriumperborat-tetrahydrat indeholdende 8¾ fugtighed.A fluidization reactor consisting essentially of a stainless steel cylindrical tube 90 mm in diameter, 0.3 kg / h sodium perborate tetrahydrate containing 8¾ of humidity is placed.

20 Den fluidiserede tilstand sikres ved hjælp af en luft strøm, hvis temperatur er 120 °C, når den træder ind i fluidiseringszonen, og hvis lineære opad stigende hastighed er 0,3 m/s.The fluidized state is ensured by an air stream whose temperature is 120 ° C as it enters the fluidization zone and whose linear upward velocity is 0.3 m / s.

Temperaturen er i fludiseringszonen 65 °C, og den relati-25 ve fugtighed er 13%.The temperature in the fludging zone is 65 ° C and the relative humidity is 13%.

Det opnåede natriumperborat-monohydrat indeholder 15,3 vægt-% aktiv oxygen, det udviser en specifik overflade 2 på 6,9 m /g, en opløsningshastighed på 100% på mindre end 1 minut samt en nedslidningsgrad på 5,8%.The sodium perborate monohydrate obtained contains 15.3% by weight of active oxygen, it exhibits a specific surface 2 of 6.9 m / g, a dissolution rate of 100% in less than 1 minute, and a wear rate of 5.8%.

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7 EKSEMPEL 2EXAMPLE 2

Idet man arbejder med det samme apparatur som beskrevet i eksempel 1; men idet man modificerer reaktionsbetingelserne som følger: - hastighed af natriumperborat-tetrahydrat med 8% fugtighed: 0,5 kg/h - temperatur af luften, som den træderUsing the same apparatus as described in Example 1; but modifying the reaction conditions as follows: - rate of sodium perborate tetrahydrate with 8% humidity: 0.5 kg / h - temperature of the air it enters

ind i fluidiseringszonen: 150 °Cinto the fluidization zone: 150 ° C

- opad stigende hastighed af gasstrøm: 0,25 m/s- upward rate of gas flow: 0.25 m / s

- temperatur i fluidiseringszonen: 70 °C- temperature in the fluidization zone: 70 ° C

- relativ fugtighed i fludiserings- zonen: 16 ?ό indeholder det således opnåede natriumperborat-monohydrat 15.4 vægt-% oxygen, det udviser en specifik overflade på 2 5.4 m /g, en opløsningshastighed på 100¾ på mindre end 1 minut og en nedslidningsgrad lig med 4,3¾.- relative humidity in the fludization zone: 16? ό contains thus obtained sodium perborate monohydrate 15.4% by weight oxygen, it has a specific surface of 2 5.4 m / g, a dissolution rate of 100¾ in less than 1 minute, and a wear rate equal to 4,3¾.

EKSEMPEL 3EXAMPLE 3

Idet man arbejdet med det samme apparatur som i eksempel 1 og 2; men idet man modificerer reaktionsbetingelserne som følger: - hastighed af natriumperborat-tetrahydrat med 8¾ fugtighed: 0,61 kg/h - temperatur af luften, som den træderWorking with the same apparatus as in Examples 1 and 2; but modifying the reaction conditions as follows: - rate of sodium perborate tetrahydrate with 8¾ humidity: 0.61 kg / h - temperature of the air as it enters

ind i fluidiseringszonen: 175 °Cinto the fluidization zone: 175 ° C

- opad stigende hastighed af gasstrøm: 0,25 m/s 8- upward rate of gas flow: 0.25 m / s 8

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- temperatur i fluidiseringszonen: 75 °C- temperature in the fluidization zone: 75 ° C

- relativ fugtighed i fluidiseringszonen 17 % indeholder det således opnåede natriumperborat-monohydrat 5 15,6 vægt-?o aktiv oxygen, det udviser en specifik over- flade på 3,3 m /g, en opløsningshastighed på 100¾ på mindre end 1 minut og en nedslidningshastighedgrad lig med 4¾.- relative humidity in the fluidization zone 17%, the sodium perborate monohydrate 5 thus obtained contains 15.6% by weight of active oxygen, exhibits a specific surface area of 3.3 m / g, a dissolution rate of 100¾ in less than 1 minute, and a wear rate equal to 4¾.

EKSEMPEL 4 10 Man anbringer i en fluidiseringsreaktor, som i hovedsa gen består af et cylindrisk rør af rustfrit stål med diameteren 300 mm, 6,3 kg/h natriumperborat-tetrahydrat indeholdende 8¾ fugtighed.EXAMPLE 4 10 A fluidization reactor consisting essentially of a cylindrical stainless steel tube 300 mm in diameter, 6.3 kg / h sodium perborate tetrahydrate containing 8¾ of humidity is placed.

Fluidiseringstilstanden sikres ved hjælp af en luftstrøm, 15 hvis temperatur er 175 °C, hvor den træder ind i fluidiseringszonen, og hvis lineære opad stigende hastighed er 0,25 m/s.The fluidization state is ensured by an air stream 15 whose temperature is 175 ° C, where it enters the fluidization zone and whose linear upward velocity is 0.25 m / s.

Temperaturerne er i fluidiseringszonen 70 °C, og den relative fugtighed er 22¾.Temperatures in the fluidization zone are 70 ° C and the relative humidity is 22¾.

20 Det således opnåede natriumperborat-monohydrat indeholder 15,25 vægt-?o aktiv oxygen, det udviser en specifik over-2 flade på 6,3 m /g, og en opløsningshastighed på 100¾ på mindre end 1 minut samt en nedslidningsgrad på 4,5¾.The sodium perborate monohydrate thus obtained contains 15.25 wt.% Of active oxygen, it exhibits a specific surface area of 6.3 m / g, and a dissolution rate of 100 mindre in less than 1 minute, and a wear rate of 4. 5¾.

EKSEMPEL 5 25 Idet man arbejder med det samme apparatur som i eksempel 4; men idet man modificerer reaktionsbetingelserne som følger:EXAMPLE 5 25 Using the same apparatus as in Example 4; but modifying the reaction conditions as follows:

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9 - hastighed af natriumperborat-tetrahydrat med 88 fugtighed: 6,7 kg/h - temperatur af luften, som den træder9 - rate of sodium perborate tetrahydrate with 88 humidity: 6.7 kg / h - temperature of the air it enters

ind i fluidiseringszonen: 175 °Cinto the fluidization zone: 175 ° C

5 - opad stigende hastighed af gasstrøm: 0,25 m/s5 - Upward rate of gas flow: 0.25 m / s

- temperatur i fluidiseringszonen: 65 °C- temperature in the fluidization zone: 65 ° C

- relativ fugtighed i fluidiseringszonen : 29 8 indeholder det således opnåede natriumperborat-monohydrat 10 15,3 vægt-8 aktiv oxygen, det udviser en specifik over- flade på 6,8 m /g, og det har en opløsningshastighed på 100?ό på mindre end 1 minut samt en nedslidningsgrad på 58.- relative humidity in the fluidization zone: 29 8 contains the thus obtained sodium perborate monohydrate 10 15.3 weight-8 active oxygen, it exhibits a specific surface area of 6.8 m / g and has a dissolution rate of 100? less than 1 minute and a wear rate of 58.

EKSEMPEL 6 15 Idet man arbejder med det samme apparatur som i eksempel 4 og 5; men idet man modificerer reaktionsbetingelserne som følger: - hastighed af natrijmperborat-tetrahydrat med 8¾ fugtighed: 8 kg/h - temperatur af luften, som den træderEXAMPLE 6 15 Using the same apparatus as in Examples 4 and 5; but modifying the reaction conditions as follows: - rate of sodium graft borate tetrahydrate with 8¾ humidity: 8 kg / h - temperature of the air as it enters

20 ind i fluidiseringszonen: 175 °C20 into the fluidization zone: 175 ° C

- opad stigende hastighed af gasstrøm: 0,4 m/s- upward rate of gas flow: 0.4 m / s

- temperatur i fluidiseringszonen 70 °C- temperature in the fluidization zone 70 ° C

- relativ fugtighed i fluidiseringszonen 22 %- relative humidity in the fluidization zone 22%

DK 163225 BDK 163225 B

10 indeholder den således opnåede natriumperborat-monohydrat 15,3 vægt-% aktiv oxygen, det udviser en specifik over-2 flade på 6,8 m /g, en opløsningshastighed på 100% på mindre end 1 minut samt en nedslidningsgrad på 6,5%.10, the sodium perborate monohydrate thus obtained contains 15.3% by weight of active oxygen, it exhibits a specific surface area of 6.8 m / g, a dissolution rate of 100% in less than 1 minute, and a wear rate of 6.5 %.

Claims (6)

1. Fremgangsmåde til kontinuert fremstilling af natrium-perborat-monohydrat ved dehydratisering af natriumperbo-rat-tetrahydrat i et enkelt trin i fluidiseret leje ved 5 hjælp af en strøm af varm luft, kendetegnet ved, at luftens temperatur er på mellem 100 °C og 180 °C, når den træder ind i fluidiseringszonen, at temperaturen i denne zone er på mellem smeltetemperaturen for natrium-perborat-tetrahydrat og 80 °C, og at den relative fugtig-10 hed er mindre end 40¾ og mindst lig med 10¾.A process for the continuous production of sodium perborate monohydrate by dehydrating sodium perborate tetrahydrate in a single step in fluidized bed by a stream of hot air, characterized in that the temperature of the air is between 100 ° C and When entering the fluidization zone, the temperature in this zone is between the sodium perborate tetrahydrate melting temperature and 80 ° C, and the relative humidity is less than 40¾ and at least equal to 10¾. 2. Fremgangsmåde ifølge krav 1, kendetegnet ved, at luftens temperatur er på mellem 130 °C og 175 °C.Process according to claim 1, characterized in that the temperature of the air is between 130 ° C and 175 ° C. 3. Fremgangsmåde ifølge krav 1 eller 2, kendetegnet ved, at den relative fugtighed er på mellem 15¾ og 15 30¾.Process according to claim 1 or 2, characterized in that the relative humidity is between 15¾ and 15¾. 4. Fremgangsmåde ifølge ethvert af kravene 1-3, kendetegnet ved, at man som bestanddel af det fremstillede produkt direkte anvender de korn, som medrives af luften uden for fluidiseringszonen, når mængden heraf 20 højst er lig med 10 vægt-?i af vægten af dannet natrium- perborat-monohydrat, uden anden behandlingsproces end deres forudgående isolering.Method according to any one of claims 1-3, characterized in that, as a component of the manufactured product, the grains entrained by the air outside the fluidizing zone are used directly when the amount thereof is not more than 10% by weight of the weight. of sodium perborate monohydrate formed, with no treatment process other than their prior isolation. 5. Fremgangsmåde ifølge krav 4, kendetegnet ved, at luftens opadgående hastighed målt under de ved 25 udgangen fra fluidiseringszonen herskende betingelser ikke overstiger 0,5 m/s.Method according to claim 4, characterized in that the upward velocity of the air measured under the conditions prevailing at the exit from the fluidization zone does not exceed 0.5 m / s. 6. Fremgangsmåde ifølge krav 4 eller 5, kendetegne t ved, at de medrevne korn isoleres ved cyklonbehand- 30 ling af den luft, der indeholder dem.Process according to claim 4 or 5, characterized in that the entrained grains are isolated by cyclone treatment of the air containing them.
DK086386A 1985-02-26 1986-02-25 PROCEDURE FOR CONTINUOUS PREPARATION OF SODIUM PERBORATE MONO HYDRATE FROM THE TETRA HYDRATE DK163225C (en)

Applications Claiming Priority (2)

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FR8503008 1985-02-26
FR8503008A FR2577916B1 (en) 1985-02-26 1985-02-26 PROCESS FOR THE CONTINUOUS MANUFACTURE OF SODIUM MONOHYDRATE PERBORATE FROM SODIUM TETRAHYDRATE PERBORATE

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IT1215566B (en) * 1987-06-17 1990-02-14 Ausimont Spa PROCESS FOR OBTAINING GRANULAR SODIUM PEROBORATE.
IT1218198B (en) * 1988-01-26 1990-04-12 Interox Chimica Spa MANUFACTURING PROCESS OF SODIUM PERBORATE MONOHYDRATE, SODIUM PERBORATE MONOHYDRATE PARTIALLY CRYSTALLIZED AND POWDERS TO SMOOTH TEXTILE MATERIALS
DE3830545A1 (en) * 1988-09-08 1990-03-15 Henkel Kgaa PROCESS FOR THE PRODUCTION OF PERBORATE
DE3941851C1 (en) * 1989-12-19 1991-06-20 Degussa Ag, 6000 Frankfurt, De
DE4316320A1 (en) * 1993-05-15 1994-11-17 Degussa Process for the production of sodium perborate monohydrate
CN100376470C (en) * 2006-09-05 2008-03-26 山东天力干燥设备有限公司 Fluidizing and drying preparing technique for sodium perborate monohydrate

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NL171507B (en) * 1952-07-30 Tektronix Inc STEP ATTENUATOR.
DE1930286B2 (en) * 1968-07-17 1979-09-06 Solvay & Cie., Bruessel Process for the production of sodium perborate monohydrate
DE2258319C3 (en) * 1972-11-29 1978-04-13 Peroxid-Chemie Gmbh, 8023 Hoellriegelskreuth Process for the production of abrasion-resistant sodium perborate monohydrate
DE2444780C2 (en) * 1974-09-19 1987-02-19 Peroxid-Chemie GmbH, 8023 Höllriegelskreuth Process for the preparation of abrasion-resistant sodium perborate monohydrate

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EP0194952B1 (en) 1988-04-06
TR22476A (en) 1987-07-22
DE3660119D1 (en) 1988-05-11
CA1256267A (en) 1989-06-27
FR2577916B1 (en) 1987-04-17
JPH0461801B2 (en) 1992-10-02
NO163853B (en) 1990-04-23
YU27586A (en) 1988-06-30
DK163225C (en) 1992-07-06
FR2577916A1 (en) 1986-08-29
DK86386A (en) 1986-08-27
IL77895A (en) 1989-07-31
EP0194952B2 (en) 1992-01-15
KR860006398A (en) 1986-09-11
EP0194952A1 (en) 1986-09-17
JPS61201605A (en) 1986-09-06
DE194952T1 (en) 1987-02-26
ES552357A0 (en) 1987-04-16
ATE33377T1 (en) 1988-04-15
NO860696L (en) 1986-08-27
NO163853C (en) 1990-08-01
AU569190B2 (en) 1988-01-21
AU5389986A (en) 1986-09-04
CN86101138A (en) 1986-08-20
ES8704851A1 (en) 1987-04-16
DK86386D0 (en) 1986-02-25
YU44542B (en) 1990-08-31

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