[go: up one dir, main page]

WO2001062664A1 - Particules de monohydrate de perborate de sodium et procede de production correspondant - Google Patents

Particules de monohydrate de perborate de sodium et procede de production correspondant Download PDF

Info

Publication number
WO2001062664A1
WO2001062664A1 PCT/GB2001/000806 GB0100806W WO0162664A1 WO 2001062664 A1 WO2001062664 A1 WO 2001062664A1 GB 0100806 W GB0100806 W GB 0100806W WO 0162664 A1 WO0162664 A1 WO 0162664A1
Authority
WO
WIPO (PCT)
Prior art keywords
sodium perborate
perborate monohydrate
particles
bulk density
weight
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.)
Ceased
Application number
PCT/GB2001/000806
Other languages
English (en)
Inventor
Igan Hayati
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
US Borax Inc
Original Assignee
US Borax Inc
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by US Borax Inc filed Critical US Borax Inc
Priority to AU2001237545A priority Critical patent/AU2001237545A1/en
Priority to EP01909959A priority patent/EP1257499A1/fr
Publication of WO2001062664A1 publication Critical patent/WO2001062664A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/39—Organic or inorganic per-compounds
    • C11D3/3942—Inorganic per-compounds
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B15/00—Peroxides; Peroxyhydrates; Peroxyacids or salts thereof; Superoxides; Ozonides
    • C01B15/055—Peroxyhydrates; Peroxyacids or salts thereof
    • C01B15/12—Peroxyhydrates; Peroxyacids or salts thereof containing boron

Definitions

  • the present invention relates to granular sodium perborate monohydrate having a high active oxygen content and a high bulk density and a method for making it. More particularly, the present invention relates to a method of manufacture which may be used to produce sodium perborate monohydrate of a high active oxygen content and high bulk density wherein the active oxygen content is in excess of 16% by weight while retaining other desirable properties that make sodium perborate monohydrate suitable as the source of hydrogen peroxide in bleaching operations in laundry detergents.
  • sodium perborates are important components and may account for up to 15% by weight of the final formulation. Both sodium perborate tetrahydrate and sodium perborate monohydrate are currently commercially available and used in the detergents industry.
  • Sodium perborate monohydrate is often favoured over sodium perborate tetrahydrate due to its high percentage active oxygen content and rapid dissolution rate in the laundry wash. Typically, a 1 g sample will dissolve in 500 ml of water at 15°C in less than one minute. However, commercially available sodium perborate monohydrate has a bulk density of around only 0.6 g/cc. It would therefore be advantageous to have a sodium perborate monohydrate with a bulk density approaching that of compact washing powders while retaining its other desirable properties. -?-
  • Sodium perborate monohydrate is commercially produced by the thermal dehydration of sodium perborate tetrahydrate. Under the processing conditions, the morphology of the sodium perborate tetrahydrate is not affected but the loss of water from the granules results in a product having a highly porous structure with an associated reduction in bulk density. Typical properties are an active oxygen content of 16% by weight, a bulk density of around 0.6 g/cc and a dissolution rate in water, as above, of less than one minute. However the product has a low attrition resistance which leads to copious amounts of fine material being produced during manufacture (typically 5-10%). These fines are usually recycled to the process for making sodium perborate tetrahydrate.
  • GB-A- 1570615 describes a process for the manufacture of granular sodium perborate monohydrate which process comprises contacting a fluidised bed containing seed particles with aqueous solutions of hydrogen peroxide and sodium metaborate and evaporating off the water.
  • the sodium perborate monohydrate is produced in situ from its precursors, hydrogen peroxide and sodium metaborate and grown on the seed particles.
  • GB-A- 1520127 describes a process in which sodium perborate tetrahydrate particles are contacted with a warm inert gas under specified conditions for removal of at least 0.8 moles of water of crystallisation.
  • US-A-4002434 describes a process for producing abrasion resistant sodium perborate monohydrate by addition of water, e.g. by spraying, in a moistening unit to preformed sodium perborate monohydrate and then drying under specified temperature conditions.
  • the water used may contain 5-10% by weight of a water- soluble material.
  • the use of a 2% hydrogen peroxide solution is exemplified. The particles, sprayed and heat treated under the conditions used, are found to become hardened and abrasion resistant.
  • US-A-4942025 describes a process for preparing granular, abrasion resistant, sodium perborate monohydrate in which, prior to its dehydration, a carboxylic acid or salt thereof is added to the starting granular sodium perborate tetrahydrate.
  • US-A-5094827 discloses the continuous production of sodium perborate monohydrate granulates by granulating primary particles produced by spraying an aqueous solution containing hydrogen peroxide and sodium metaborate into a hot gas and drying.
  • the sodium perborate primary particles are granulated in the presence of a granulating agent which ma ⁇ ' be water or sodium perborate tetrahydrate.
  • Hydrogen peroxide inter alia is mentioned as a possible additive to the water.
  • US-A-5395602 describes a compaction method whereby sodium perborate monohydrate having a low bulk density is compacted between rollers at a contact pressure of 5x10 3 to 2x10 4 N/cm.
  • the shells so produced are comminuted and sieved according to particle size.
  • the present invention concerns the obtaining of sodium perborate of increased active oxygen content and bulk density by agglomeration using concentrated hydrogen peroxide solution as agglomerating agent.
  • sodium perborate monohydrate particles of high active oxygen content and also high bulk density may be obtained by agglomeration using a high concentration hydrogen peroxide solution as agglomeration agent. This process may be used for the agglomeration of the fines obtained in the manufacture of sodium perborate monohydrate b ⁇ dehydration of sodium perborate tetrahydrate.
  • the invention also provides the agglomerated particles obtained by the method of the invention.
  • the sodium perborate monohydrate particles which are treated are the fines produced as undersized materials in the manufacture of sodium perborate monohydrate by the dehydration of sodium perborate tetrahydrate.
  • Such fines typically have an active oxygen content in the region of 15% by weight and a bulk density in the region of 0.6 g/cc.
  • the sodium perborate monohydrate particles to be agglomerated typically have a particle size of less than 350 ⁇ m.
  • a significant proportion of the starting particles may be below 45 ⁇ m in size. However generally the majority of the starting particles will be in the range 45 to 300 ⁇ m. more particular 125 to 300 ⁇ m. and preferably 180 to 250 ⁇ m.
  • the agglomerates obtained according to the invention are 90 to 710 ⁇ m in size. The final agglomerate size will, naturally, depend amongst other things on the starting particle size.
  • the starting sodium perborate monohydrate particles will normally have a bulk density in the region of 0.55 to 0.65 g/cc.
  • the final agglomerates obtained according to the invention may have a bulk density above 0.7 g/cc, e.g. 0.7 to 0.9 g/cc.
  • the agglomerating agent used is suitably an aqueous 20 to 80% weight by volume hydrogen peroxide solution.
  • agglomerating agent an aqueous hydrogen peroxide solution having a concentration of at least 30%o weight by volume and the upper limit may generally be 70% weight by volume.
  • agglomerating agent an aqueous 30 to 60%o weight by volume hydrogen peroxide solution.
  • a further advantage of the invention is that the agglomerated particles obtained are generally more resistant to attrition than the irregularly shaped particles of commercially available sodium perborate monohydrate as the effect of agglomeration is to produce particles substantially spherical in shape and having a smooth surface instead of a dendritic particle shape.
  • the spherical particle shape ensures better packing, which together with the reduced porosity of the product, results in a higher bulk density over sodium perborate monohydrate manufactured by conventional means.
  • sodium perborate monohydrate particles in a finely divided state produced as undersized material in the manufacture of sodium perborate monohydrate by the dehydration of sodium perborate tetrahydrate and having an active oxygen content of 15% by weight and a bulk density of about 0.6g/cc may in particular be agglomerated to increase their active oxygen content and bulk density in the presence of an agglomerating agent comprising at least 30% weight by volume aqueous hydrogen peroxide solution followed by drying.
  • particles of fine sodium perborate tetrahydrate are manufactured by means known to those skilled in the art, e.g. by adjusting the crystallisation conditions to obtain fine particles having a particle size generally less than 350 ⁇ m. These are then partially or fully dehydrated and may be agglomerated to increase their active oxygen content and bulk density in the presence of an agglomerating agent comprising at least 30% weight by volume aqueous hydrogen peroxide solution followed by drying.
  • the starting sodium perborate monohydrate particles may have an active oxygen content of 15 to below 16% by weight, while the agglomerated product will have an active oxygen content of at least 16 % e.g. 17, to 19.5%) by weight, such as 16 to 18%> by weight.
  • sodium perborate monohydrate having a particle size less than 350 ⁇ m and an active oxygen content of 15.5 % by weight granulated by spraying with 30%o weight by volume hydrogen peroxide solution and oven dried, was found to have an increased bulk density to 0.77 g/cc due to better packaging and reduced porosity, and an active oxygen content of 16.7% by weight.
  • an agglomerating agent containing up to 60%> weight by volume of hydrogen peroxide may be used. Amounts below 30%> do not generally significantly affect the overall increase in bulk density of the sodium perborate monohydrate nor the particle shape and the effects of improvements in active oxygen content are diminished.
  • the agglomeration according to the invention may be carried out in a conventional manner by adding the hydrogen peroxide in the form of a fine spray.
  • the granulating device used may be any apparatus suitable for the mixing of dry paniculate materials adapted so that a liquid granulating agent can be sprayed on or otherwise added to the particles.
  • Conventional granulation equipment can be used.
  • An intensive mixer such as an Eirich mixer, may be used.
  • the desired agglomerated product is obtained.
  • Undersize and/or oversize particles can be removed, for instance by screening, if a narrow particle size distribution is desired for the agglomerated product. This may be desirable as coarser particles have a higher active oxygen content.
  • the oversize can be crushed and recycled.
  • the time required for agglomeration is dependent on the rate at which the hydrogen peroxide solution is added and the speed of agitation.
  • a suitable agglomeration time is about 15 minutes when using a laboratory size batch mixer.
  • agglomerator residence times may be much shorter e.g. a matter of a few seconds.
  • the hydrogen peroxide solution is suitably used in an amount of about 14% by weight based on the total weight of the particles. It is sprayed through fine jets directly onto the material being mixed in a granulating device at ambient temperature of about 15°C to 25°C.
  • the droplet size is suitably about 50 microns.
  • the product is dried. Drying is conveniently carried out in a fluid bed drier operating at about 50°C with a typical residence time of about 30 minutes.
  • the sodium perborate monohydrate granulated product prepared in accordance with the invention dissolves very rapidly in water. The rate of dissolution is consistent with that desired for products being incorporated into detergent formulations.
  • the dissolution rates can be controlled by methods well known in the art by the inclusion of highly soluble materials, surfactants or disintegrants or by coating with slowly dissolving materials.
  • the active oxygen content of the sodium perborate monohydrate obtained according to the invention has been found to be stable on standing in the open at ambient temperature for six weeks.
  • the attrition index of the sodium perborate monohydrate according to the mvention according to ISO Test 5937 is generally less than 10%) and the bulk density above 0.7 g/cc.
  • the invention further provides detergent compositions containing sodium perborate monohydrate particles according to the invention and the use of those particles in detergent compositions.
  • the detergent compositions may contain a surfactant, for example, an anionic surfactant such as an alcohol sulphate or linear alkyl benzene sulphonate and/or non- ionic surfactants, such as an alcohol ethoxvlate.
  • a surfactant for example, an anionic surfactant such as an alcohol sulphate or linear alkyl benzene sulphonate and/or non- ionic surfactants, such as an alcohol ethoxvlate.
  • the detergent compositions will generally contain builders such as aluminosilicates (e.g. zeolite A), layered silicates, phosphates particularly sodium tripolyphosphate, trisodium citrate, sodium carbonate or sodium borate.
  • polymeric additives such as maleic/acrylic copolymers which act as co-builders, and soil release polymers such as polyethylene oxide terephthalate.
  • the detergent compositions may also contain suds suppressors such as soap; enzymes such as lipase, amylase, cellulase and protease; optical brighteners such as stilbe e derivatives, sequestrants and flow aids/fillers such as sodium sulphate.
  • suds suppressors such as soap
  • enzymes such as lipase, amylase, cellulase and protease
  • optical brighteners such as stilbe e derivatives, sequestrants and flow aids/fillers such as sodium sulphate.
  • the sodium perborate monohydrate particles according to the invention have particular use in detergent tablet formulations, which may be single- or multi-layered, consisting of compressed particulate detergent ingredients. These may be used in laundry or dishwashing applications.
  • Sodium perborate monohydrate fines (3000g) having a particle size less than 350 ⁇ m, an active oxygen content of 15% by weight and bulk density of 0.6 g/cc were charged into an Eirich mixer and agitated at 1300 rpm. 30%) weight by volume hydrogen peroxide solution (420g) was sprayed directly onto the fines through an ultrasonic sprayer at a rate of 30 ml per minute.
  • the mixer was stopped and the product was transferred to a fluid bed dryer operating at 50°C for a period of 30 minutes.
  • the product was a free-flowing granular material having the appearance of sodium perborate monohydrate manufactured by conventional means. On microscopic examination, the individual particles were seen to have smooth surfaces. The % active oxygen by weight was measured at 16.7 and the bulk density was 0.77 g/cc.
  • Example 1 The method of Example 1 was followed except that 60% weight by volume hydrogen peroxide solution was used instead of 30%.
  • Example 2 The product was similar in appearance to that of Example 1.
  • the % active oxygen by weight was measured at 17.8 and the bulk density was 0.77 g/cc.
  • Milled ( ⁇ 75 ⁇ ) sodium perborate monohydrate (active oxygen by weight 15.3%) and 60%) weight by volume hydrogen peroxide solution were added continuously to a continuous granulator at a liquid to powder ratio of 15.3%) by weight. The rate of addition was 500 kg per hour.
  • the wet agglomerates were then passed through a fluid bed drier where they were dried at 40°C and cooled to 25°C over a period of 30 minutes.
  • Example 2 The product was similar in appearance to that of Example 1.
  • the % active oxygen by weight was measured at 19.2 and the bulk density was 0.78 g/cc.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Detergent Compositions (AREA)

Abstract

L'invention concerne un procédé de production de monohydrate de perborate de sodium possédant une teneur élevée oxygène actif et une forte densité volumique, et de particules de perborate de sodium pouvant être produites au moyen dudit procédé. Selon l'invention, ce procédé comprend l'agglomération de fines particules de perborate de sodium utilisant comme agent d'agglomération une eau oxygénée à concentration élevée, puis le séchage. Le produit obtenu possède les propriétés souhaitées d'un monohydrate de perborate de sodium disponible sur le marché, mais aussi, notamment, une teneur élevée en oxygène actif et une forte densité volumique qui le rend utile dans des formulations de détergents dites compactes ou super compactes.
PCT/GB2001/000806 2000-02-24 2001-02-23 Particules de monohydrate de perborate de sodium et procede de production correspondant Ceased WO2001062664A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
AU2001237545A AU2001237545A1 (en) 2000-02-24 2001-02-23 Sodium perborate monohydrate particles and their manufacture
EP01909959A EP1257499A1 (fr) 2000-02-24 2001-02-23 Particules de monohydrate de perborate de sodium et procede de production correspondant

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
GB0004406A GB2359546A (en) 2000-02-24 2000-02-24 Agglomerating sodium perborate monohydrate particles
GB0004406.5 2000-02-24

Publications (1)

Publication Number Publication Date
WO2001062664A1 true WO2001062664A1 (fr) 2001-08-30

Family

ID=9886341

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/GB2001/000806 Ceased WO2001062664A1 (fr) 2000-02-24 2001-02-23 Particules de monohydrate de perborate de sodium et procede de production correspondant

Country Status (4)

Country Link
EP (1) EP1257499A1 (fr)
AU (1) AU2001237545A1 (fr)
GB (1) GB2359546A (fr)
WO (1) WO2001062664A1 (fr)

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DD114051A1 (fr) * 1974-08-02 1975-07-12
US3975500A (en) * 1974-08-29 1976-08-17 E. I. Du Pont De Nemours And Company Process for producing high active oxygen, low bulk density sodium perborate
US4185960A (en) * 1977-04-08 1980-01-29 Interox Super-oxidized solid sodium perborate and processes for its manufacture
EP0328768A1 (fr) * 1988-02-13 1989-08-23 Degussa Aktiengesellschaft Procédé continu pour la confection de granules de perborate de sodium
US5395602A (en) * 1989-12-19 1995-03-07 Degussa Aktiengesellschaft Method for the production of sodium perborate hydrate granulates

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2203285A1 (de) * 1972-01-25 1973-08-16 Degussa Verfahren zur herstellung von abriebfestem perboratmonohydrat
LU73751A1 (fr) * 1975-11-06 1977-06-03

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DD114051A1 (fr) * 1974-08-02 1975-07-12
US3975500A (en) * 1974-08-29 1976-08-17 E. I. Du Pont De Nemours And Company Process for producing high active oxygen, low bulk density sodium perborate
US4185960A (en) * 1977-04-08 1980-01-29 Interox Super-oxidized solid sodium perborate and processes for its manufacture
EP0328768A1 (fr) * 1988-02-13 1989-08-23 Degussa Aktiengesellschaft Procédé continu pour la confection de granules de perborate de sodium
US5395602A (en) * 1989-12-19 1995-03-07 Degussa Aktiengesellschaft Method for the production of sodium perborate hydrate granulates

Also Published As

Publication number Publication date
GB2359546A (en) 2001-08-29
EP1257499A1 (fr) 2002-11-20
AU2001237545A1 (en) 2001-09-03
GB0004406D0 (en) 2000-04-12

Similar Documents

Publication Publication Date Title
EP0292314B1 (fr) Procédé pour encapsuler des particules utilisant un latex de polymère
KR920000114B1 (ko) 세제조성물 및 그 제조방법
JPH0759719B2 (ja) 嵩密度の高い粒状洗剤組成物の製法
JPH04227700A (ja) 高嵩密度顆粒状洗剤組成物及びその製造方法
JPS62112697A (ja) 洗剤組成物、その成分、およびその製造方法
RO110261B1 (ro) Agent adjuvant activ, pe baza de silicat de metal alcalin si de produs mineral si procedeu de obtinere a acestuia
EP2585572A1 (fr) Particules revêtues contenant un agent chélatant à base de n,n-diacétate d'acide glutamique
CA2782583A1 (fr) Particules revetues d'un agent chelatant a base de n,n-diacetate d'acide glutamique
JPH04501129A (ja) 界面活性剤含有顆粒の製法
CN113767153B (zh) 作为用于释放家用护理制剂中的一种或更多种活性剂的载体材料的经表面反应的碳酸镁
US20040224874A1 (en) Process for producing coated detergent particles
CA1303939C (fr) Poudres detergentes et procede de fabrication connexe
CN102858936B (zh) 包含过碳酸钠和漂白活化剂的漂白剂颗粒
JPH07106891B2 (ja) 珪酸塩顆粒の製造方法
AU5549198A (en) Method to produce sodium percarbonate
WO2012000914A1 (fr) Particules pourvues d'un revêtement comportant un (co)polymère d'alcool vinylique et un polysaccharide
HU217766B (hu) Eljárás kis relatív nedvességtartalmú detergens kompozíció előállítására és detergens kompozíciók
EP1257499A1 (fr) Particules de monohydrate de perborate de sodium et procede de production correspondant
CA1337041C (fr) Compositions granulaires de detergent, a solubilite amelioree
HUP0202354A2 (en) Particulate detergent composition containing zeolite
EP1232238B1 (fr) Procede de preparation de compositions detergentes granulaires
EP1953217B1 (fr) Additif granulé utilisé dans les compositions détergentes
JPH06504303A (ja) 洗剤の成分を含有する易溶解性の乾燥濃厚物
JP2008519115A (ja) 洗剤または洗浄剤のための顆粒／凝集物
JPH02217313A (ja) 改良されたゼオライト組成物

Legal Events

Date Code Title Description
AK Designated states

Kind code of ref document: A1

Designated state(s): AE AG AL AM AT AU AZ BA BB BG BR BY BZ CA CH CN CR CU CZ DE DK DM DZ EE ES FI GB GD GE GH GM HR HU ID IL IN IS JP KE KG KP KR KZ LC LK LR LS LT LU LV MA MD MG MK MN MW MX MZ NO NZ PL PT RO RU SD SE SG SI SK SL TJ TM TR TT TZ UA UG US UZ VN YU ZA ZW

AL Designated countries for regional patents

Kind code of ref document: A1

Designated state(s): GH GM KE LS MW MZ SD SL SZ TZ UG ZW AM AZ BY KG KZ MD RU TJ TM AT BE CH CY DE DK ES FI FR GB GR IE IT LU MC NL PT SE TR BF BJ CF CG CI CM GA GN GW ML MR NE SN TD TG

121 Ep: the epo has been informed by wipo that ep was designated in this application
DFPE Request for preliminary examination filed prior to expiration of 19th month from priority date (pct application filed before 20040101)
WWE Wipo information: entry into national phase

Ref document number: 2001909959

Country of ref document: EP

WWP Wipo information: published in national office

Ref document number: 2001909959

Country of ref document: EP

WWW Wipo information: withdrawn in national office

Ref document number: 2001909959

Country of ref document: EP

REG Reference to national code

Ref country code: DE

Ref legal event code: 8642

NENP Non-entry into the national phase

Ref country code: JP