[go: up one dir, main page]

CN1046932A - Agglomerated granular peroxyacid bleach and process for its preparation - Google Patents

Agglomerated granular peroxyacid bleach and process for its preparation Download PDF

Info

Publication number
CN1046932A
CN1046932A CN 90102598 CN90102598A CN1046932A CN 1046932 A CN1046932 A CN 1046932A CN 90102598 CN90102598 CN 90102598 CN 90102598 A CN90102598 A CN 90102598A CN 1046932 A CN1046932 A CN 1046932A
Authority
CN
China
Prior art keywords
heat release
peroxyacid bleach
synthetic optical
control agent
optical whitner
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
Application number
CN 90102598
Other languages
Chinese (zh)
Inventor
查尔斯·爱德华·凯尔纳
史蒂文·罗伯特·亚历山大
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.)
Procter and Gamble Co
Original Assignee
Procter and Gamble Co
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 Procter and Gamble Co filed Critical Procter and Gamble Co
Publication of CN1046932A publication Critical patent/CN1046932A/en
Pending 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
    • C11D3/3945—Organic per-compounds
    • 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
    • C11D3/3902—Organic or inorganic per-compounds combined with specific additives
    • C11D3/3937—Stabilising agents
    • 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
    • C11D3/3902—Organic or inorganic per-compounds combined with specific additives
    • C11D3/3937—Stabilising agents
    • C11D3/394—Organic compounds

Landscapes

  • Chemical & Material Sciences (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)
  • Organic Chemistry (AREA)
  • Detergent Compositions (AREA)

Abstract

本发明涉及一种干粒状过氧酸漂白剂组合物及制造它的新方法，该方法包括：在适当的混合器中将湿的过氧酸漂白剂喷涂在干的粒状固体上，形成湿的漂白剂颗粒产品，在控制条件下于流化床干燥器中将其干燥。The present invention relates to a dry granular peroxyacid bleach composition and a novel method of making the same, the method comprising: spraying wet peroxyacid bleach in a suitable mixer onto a dry granular solid to form a wet Bleach granular product, which is dried under controlled conditions in a fluid bed dryer.

Description

Peroxyacid bleach granule of reuniting and preparation method thereof
The present invention relates to peroxyacid bleach granule and the hygroscopicity mixture of being made up of peroxyacid bleach and heat release control agent is changed into the method for stable dried particles.
Disclosed the composition that contains peroxy acid and heat release control agent in the bibliography that prior art comprises.At United States Patent (USP) 4,170,453(1979 October 9, usually mentioned in Kitko) and prepared peroxyacid bleach granule with agglomeration process.But this patent is not discussed advantage, shortcoming or detail with agglomeration process.
At the common United States Patent (USP) of transferring the possession of 4,497,757(1985 February 5 disclosed the low-density peroxyacid bleach particle of preparation in spray tower in Beimesch/Hortel), this patent is here quoted as a reference.Other background information is a United States Patent (USP) 3,703,772(1972 November 28, McHugh etc.) and its with United States Patent (USP) 4,091 of transferring the possession of, 544(1978 May 30, Hutchins), the two is all here quoted as a reference.The method of these prior arts needs several extra steps to obtain the peroxyacid bleach granule of higher density.
The present invention relates to a kind of dried, peroxyacid bleach granule composition and its a kind of new preparation method, comprising: in suitable mixing tank, under the condition of control, wet peroxyacid bleach is sprayed on the dry granular component of exsiccant whitener composition.
The granular bleaching agent that the invention provides a kind of drying and reunite, it is peroxyacid bleach and peroxyacid bleach heat release control agent solid compounding mixture, the quantity of heat release control thing has been enough to stabilization.The present invention also provides the method for the granular bleaching agent of preparation reunion.
" reunion " speech here refers to form particle with coating, bonding and blended method, comprises forming doughy intermediate and composition thereof.
Particle of the present invention has complicated crystalline state, its structure and prior art, for example aforesaid United States Patent (USP) 4,091,544 and 4,497, the spheroidal particle disclosed in 757 or flap difference.
Method of the present invention is saved energy than prior art, guarantees that bleach particle has homogeneity preferably, not heat release when removing moisture by wet peroxyacid bleach intermediate, and it is less to degrade simultaneously.
Method of the present invention may further comprise the steps:
A. make a kind of pumpable, preferably sprayable, the hygroscopicity slurry, it contains:
(1) about water of 26% to 55%;
(2) about peroxyacid bleach of 20% to 45%;
(3) be at least about 1/3 the peroxy acid heat release control agent that has been enough to stabilization quantity;
B. in mechanical mixer with the wet pulp body pumping in the steps A or spray in the incoming flow of exsiccant granular solids, form wet bleach particle, to contain remaining above-mentioned heat release control agent in the granular solids of incoming flow at least; Wet bleach particle free water content in this step is about 10% to 20%;
C. the SYNTHETIC OPTICAL WHITNER wet granular among the step B is dried to final free water content under the temperature of control and is lower than about 0.5%.
It is about 0.5% that the particulate free water content is lower than, to have stability and flowable.Particulate density of the present invention is at least about 0.5 gram/cubic centimetre.Preferably from about 0.6 to 0.7 gram/cubic centimetre.The particle that prior art makes with comminution granulation, its density are 0.35 to 0.45 gram/cubic centimetre, far below 0.5 gram/cubic centimetre.Particulate free water content of the present invention is preferably from about 0.1% to 0.3%.
Optimum water concentration in the steps A is from about 30% to 40%.Optimum water concentration among the step B is from about 12% to 18%.The final free water content of particulate is preferably from about 0.1% to 0.3% among the step C.
In continuous processing, the average mixing time of step B is very short, preferably from about 0.2 second to 5 seconds.
Step C the fluidised bed drying time preferably from about 10 minutes to 60 minutes.Dry air inlet optimum temps is about 35 ℃ to 100 ℃ among the step C, keeps the temperature of wet granular to be lower than 60 ℃ simultaneously.
" temperature of control " among the step C is meant that temperature is lower than the unstability temperature of SYNTHETIC OPTICAL WHITNER.
In the steps A the preferred temperature of slurry be from about 30 ℃ to the highest about 40 ℃.The better service temperature of steps A is from about 34 ℃ to 38 ℃, and step C then is from about 38 ℃ to 82 ℃.Drying is preferably in the fluidized bed dryer carries out.
Here used " pumpable " speech is meant that slurry can contain in the mechanical mixer of dry granular component with logistics or Sprayable introducing.
The content of the peroxyacid bleach in the exsiccant bleach particle is about the 10% to 35% better of particle weight, preferably from about 20% to 30%.
Peroxyacid bleach
Peroxy acid can be with any suitable peroxy acid.At United States Patent (USP) 4,374,035(1983 February 15 F.P.Bossu) and United States Patent (USP) 4,770,666(1988 September 13 disclosed the organic peroxide acid that is suitable in A.D.Clauss), the two is incorporated herein by reference.
The consumption of peroxyacid bleach should be able to provide approximately from 0.1% to 10% available oxygen (AvO), and from 0.5% to 5% is better, and preferably roughly from 1% to 4%.Contain 1% to 50% heat release control agent (for example boric acid) in the preferred granular bleaching agent, 3% to 25% can be compatible with peroxy acid tensio-active agent (C for example 13LAS), one or more chelate stabilizers of 0.01% to 10% (for example trisodium phosphate), 10% to 50% water-soluble refined salt (Na for example 2SO 4).
A kind of preferred peroxyacid bleach, its consumption can provide about available oxygen of 1.2% to 5% (AvO), and from 2% to 4% better, preferably from about 2.5% to 3.5%.
A kind of preferred peroxy acid of using in present method is to be generally the solid peracetic acid compound.If compound is exsiccant or solid form at room temperature, then be " being generally solid ".This class peracetic acid compound is organic peroxide acid and water-soluble salt thereof, and its aqueous solution resultant contains-the O-O-group.The general formula of these materials is
Wherein R contains 1 alkylidene group or phenylene to about 20 carbon atoms, and Y is hydrogen, halogen, alkyl, aryl or anyly can generates anionic group in the aqueous solution.These Y groups can comprise, for example,
Wherein M is H or water-soluble salt-forming cation.
The aromatics peroxy acid that is suitable for and the example of salt thereof comprise single sodium salt, metachloroperbenzoic acid of monoperphthalic acid, two peroxide terephthalic acid, the two peroxide phthalic acids of 4-chlorine, two peroxide terephthalic acids, to nitro benzoyl hydroperoxide and two peroxide m-phthalic acid.What override was selected for use in present method is that two peroxide dodecandioic acids, nonyl acid amides are crossed oxydisuccinic acid (NAPSA) and two peroxide nonane diacid.
Peroxy acid heat release control agent
The peroxy acid wet mixture of preparation process A reduces the water-content of peroxy acid wet mixture in step B, and in step C with wet bleach particle drying, all these operations all need careful.Preferably in drying step C, remove all moisture in the wet granular basically, but so that improve the oxygen supply stability of peroxy acid.Necessary controlled step A and the mixing temperature of B and the air themperature of mix ingredients and step C will make temperature reach the temperature that heat release takes place or significantly degrade scarcely.Therefore, must take measures to guarantee that mixing and drying temperature do not make the peroxy acid exothermic decomposition.For helping to control the heat release problem, in mixture, add a kind of reagent, it can disengage moisture about the heat release point of SYNTHETIC OPTICAL WHITNER, thus the control heat release.This class reagent will be discussed below.
Thickness and the drying means of the time of standing drying temperature with selected temperature, material, individual particle becomes, but normally from about several minutes to several hours, drying temperature is from about 25 ℃ to 100 ℃, preferably from about 60 ℃ to 70 ℃, as long as the temperature of bleach particle itself is no more than about 60 ℃.The temperature of exsiccant bleach particle preferably keeps below about 55 ℃.
Used actual device can be any coarctate device of particle that can not make in the last drying.Terminology used here " fluidized bed dryer " comprises the air blast through circulation dryer of travelling belt drying machine (air blast air cycle) and any kind of, (the Ft.Lee of Wyssmont company for example, New Jersey) Gong Ying Wyssmont turbodrier, they can be used for dry wet bleach particle of the present invention.
In the peroxy acid document, extensively put down in writing peroxy acid to various stability problem sensitivities, also may cause some problem.A bit, the peroxy acid exothermic decomposition when material is in the dry granular form, must be controlled to guarantee product safety the heat that produces after considering earlier.Best heat release control agent is those control agents that can discharge moisture a little less than the decomposition temperature of used peroxy acid the time.United States Patent (USP) 3,770 Nielsen) discloses many kinds of hydrates at 816(1973 November 6, is suitable as the heat release control agent, and described patent is incorporated herein by reference.Comprise bitter salt, Magnesium Formate Dihydrate, calcium sulfate (CaSO in these materials 42H 2O), hydration calcium lactate, calcium sulfate sodium (CaSO 42Na 2SO 42H 2O) and the hydrate that resembles this class material of aluminium sodium sulfate, potassium aluminium sulfate, exsiccated ammonium alum and Tai-Ace S 150.Preferred hydrate is a Tai-Ace S 150 basic metal, and preferred especially person is a potassium aluminium sulfate.Other heat release control agent comprises " hydrate " of other acceptable acid addition salts.Preferred heat release control agent is owing to decomposition and those materials of dehydration, for example boric acid, oxysuccinic acid and toxilic acid.
The heat release control agent preferably uses with the consumption that can play stabilization, and 70% to 400%, 75% to 200% of being approximately peracetic acid compound weight is better, preferably is about 100% to 150%, and this will decide according to the type of used peracetic acid compound and control agent.
Compare with preferred heat release control agent, some kind in these materials needs more quantity could control heat release.
Other material
When using peracetic acid compound, the other problem that runs into belongs to the scope that good bleaching is renderd a service of how keeping.Have recognized that metal ion can play catalyst action in the degraded of peracetic acid compound.For overcoming this problem, can add 0.005% to 1% the sequestrant that consumption is about composition weight, with the constraint heavy metal ion.United States Patent (USP) 3,442,937(1969 May 6, Sennewald etc.) a kind of sequestrant system is disclosed, the urea (optional) that contains quinoline or its salt, alkali metal polyphosphates and play synergistic amounts.United States Patent (USP) 2,838,459(1958 June 10, Sprout Jr) discloses many kinds of polyphosphate, can be used as the stablizer that superoxide is bathed.These materials can be in the present invention as stabilization aid.United States Patent (USP) 3,192, Cann) discloses with quinardinic acid and has stablized percarboxylic acids 255(1965 June 29.This material, and pyridine carboxylic acid and oxine also can be used in the composition of the present invention.A kind of preferred chelating system of the present invention is pyridine dicarboxylic acid and acid polyphosphate, the mixture of sodium acid pyrophosphate preferably.The acid polyphosphate can be the mixture of phosphoric acid and trisodium phosphate, and wherein the ratio of the former with the latter is about 0.5: 1 to 2: 1, and the ratio of this mixture and pyrrole shallow lake dicarboxylic acid is about 0.2: 1 to 5: 1.
Other reagent that can be used for improving bleachability comprises pH regulator agent, bleach-activating agent and accessory Synergist S-421 95, for example tinting material, dyestuff and spices.Typical pH regulator agent is to be used for the pH of this composition solution is changed to or maintain 5 to 10 scope, and peroxyacid bleach is the most effective usually in this scope.The pH regulator agent can be an acid type, also can be the alkali type, and this depends on the character of other optional components of composition.The purpose of acidic ph modifier is the existence of other high alkalinity material of compensation, and the example comprises and is generally solid organic acid and mineral acid, the mixture of acid, and acid salt.The example of this class acid type pH regulator agent has citric acid, oxyacetic acid, tartrate, glyconic acid, L-glutamic acid, thionamic acid, sodium pyrosulfate, sal enixum, monoammonium sulfate and citric acid and lauric mixture.Citric acid is preferentially selected for use because of its hypotoxicity and rigid sequestering power.
Optional alkali type pH regulator agent comprises conventional ealkaline buffer.The example of this class buffer reagent has carbonate, supercarbonate, silicate, pyrophosphate salt and their mixture.Preferably use sodium bicarbonate and tetrasodium pyrophosphate.
These nonessential optional components, if be used to form final SYNTHETIC OPTICAL WHITNER product with active peroxy acid of the present invention/heat release control agent system, they constitute 50% to 95% of composition total weight approximately.On the contrary, bleach systems constitutes 5% to 50% of composition approximately.Optional components resemble the metal chelator is preferably mixed with peroxy acid and heat release control agent in steps A or B mutually, thereby becomes the dry part of the whole that work in-process generates.Other component, for example pH regulator agent, then the form with separating particles adds in step B, or mixes mutually with particulate matter of the present invention.If other component of this class may cause the peroxy acid degraded, then can it be applied with for example inertia fatty substance.
Above-mentioned bleaching composition can be added to a part that constitutes it in the fabric detergent composition commonly used.Therefore, the optional components of bleaching composition of the present invention can comprise as tensio-active agent and the such washing composition auxiliary of washing assistant.Optional tensio-active agent is optional from organic anionic, non-ionic type, amphoteric and amphoteric ionic surfactant and their mixture.Optional washing assistant comprises any organic washing-assisting detergent salt commonly used, as carbonate.
The water-soluble salt of higher fatty acid, i.e. " soap " can be used for the present invention and makes anion surfactant.
The anion surfactant of other class comprises the water-soluble salt of organic sulfating reaction product; especially basic metal, ammonium and alkanol amine salt have an alkyl that contains about 8 to 22 carbon atoms and sulfonic acid or sulfate group (" alkyl " comprises the moieties of acyl group) in its molecular structure.
The preferred water soluble anion organic surface active agent of the present invention comprises linear alkylbenzene sulfonate, and its alkyl contains about 11 to 14 carbon atoms; The alkyl-sulphate of tallow scope; The alkyl glycerol sulfonate of Oleum Cocois scope; And alkyl ether sulphate, moieties wherein contains about 14 to 18 carbon atoms, and average degree of ethoxylation is 1 to 6.
Being used for particularly preferred anion surfactant of the present invention comprises: straight chain C 10-C 12Sodium alkyl benzene sulfonate; C 10-C 12The alkyl benzene sulphonate (ABS) trolamine; Tallow alkyl sodium sulfate; Coconut alkyl glycerylether sodium sulfonate; Sodium salt with the sulfation condensation product of tallow alcohol and about 3 to 10 moles of ethylene oxide.
Above-mentioned any anion surfactant can use respectively in the present invention, also can use with the form of mixture.
The granular composition for preparing can also contain those washing auxiliary detergents that are usually used in the cleaning composition.The available washing assistant comprises any inorganic and organic water-soluble builder salt commonly used among the present invention, and various water-insoluble and so-called " seeding formula " washing assistant.
The available inorganic builders comprises, water-soluble phosphate, pyrophosphate salt, orthophosphoric acid salt, polyphosphate, phosphonate, carbonate, supercarbonate, borate and silicate.United States Patent (USP) 3,159 discloses these and other phosphorous washing-aid compound in 581,3,213,030,3,422,021,3,422,137,3,400,176 and 3,400,148, and described patent is quoted as a reference here.Tripoly phosphate sodium STPP is particularly preferred water-soluble inorganic washing assistant.
Also can select for use not the phosphorated sequestrant as washing auxiliary detergent.The specific examples of the inorganic builders of non-phosphorus comprises water-soluble inorganic carbonate, supercarbonate, borate and silicate.Basic metal, for example, the carbonate of sodium and potassium, supercarbonate, borate (borax) and silicate are particularly useful.
Also can use water-soluble organic washing-assisting detergent.
The non-phosphorus Cleaning Aid Agent of especially preferentially selecting for use (inorganic and organically) comprises yellow soda ash, sodium bicarbonate, water glass, Trisodium Citrate, oxygen di-sodium succinate, these six sodium formiates, sodium nitrilo triacetate and sodium ethylene diamine tetracetate, and their mixture.
The another kind of washing auxiliary detergent that can be used in the present composition and the method comprises a kind of a kind of crystal seed that can form the water-soluble substances of water-fast reaction product and cooperate with it with rigid positively charged ion in the water, and this crystal seed provides growth site for described reaction product.
Also having a class available washing assistant is various water-fast basically materials, and they can reduce the hardness of washings by for example ion exchange process.
Smecta, promptly the zeolite type material can be used as pre-stain/washing adjuvant, and these materials energy softening waters are promptly removed rigid Ca ++Ion.Natural and synthetic " zeolite ", particularly zeolite A and aquation zeolite A all can be used as washing assistant/tenderizer.At United States Patent (USP) 2,882,243(1959 April 14 mentioned zeolite-like materials and preparation method thereof in Milton), this patent is here quoted as a reference.
Granular bleaching agent of the present invention can be used with the dirt agent for releasing.Available dirt agent for releasing is included in those disclosed kind in the above-mentioned United States Patent (USP) 4,770,666, quotes as a reference here.
Any dry-matter that uses as " dryer feed " part in step B comprises remaining heat release control agent, washing assistant etc., except as otherwise noted, all is referred to as " filler " here.
Peroxyacid bleach particle of the present invention can with other compatible granular bleaching agent and/or detergent composition fusion mutually.Contain the particle of SYNTHETIC OPTICAL WHITNER or the granular size of nonessential optional saccharoid and do not have strict regulation.But the certain particle scope is preferably arranged so that have commercial gratifying flowing property.Therefore, for well, 100 microns to 1300 microns then better, preferably from about 250 microns to 1000 microns between about 100 microns to 3000 microns for the granular size of the present composition.
When using bleaching composition of the present invention that it is soluble in water, its quantity should be enough to provide the available oxygen of about 1.0ppm to 100ppm in solution.Usually, this is equivalent to 0.01% to the 0.2%(weight of having an appointment in the solution) composition.Fabric with the desire bleaching contacts with aqueous bleaching solution then.
Following example has illustrated dry granular shape peroxy acid bleach composition and method of making the same of the present invention, but the invention is not restricted to this.Percentage ratio and umber are all by weight.
Example 1
Prepare dry granular shape peroxyacid bleach composition with following material:
Peroxyacid bleach wet pulp body umber
Two peroxide dodecandioic acids (DPDA) 22.9%; 0.93
Water 46%; Boric acid 25.2%; Surfactivity
Agent slurry+accessory constituent 5.9%
The dryer feed solid
Anhydrous sodium sulphate 0.35
The dried fine powder 2.95 of the DPDA of recirculation
Amount to 4.32
Used equipment is the Aeromatic intermittent type STREA-1 type fluidized bed dryer that 8 inches TC of Bepex, 8 Turbulizer mixing tanks and AeromaticAG company (Muttenz) make.
Steps A
Boric acid and tensio-active agent slurry+accessory constituent are added in the aqueous solution of two peroxide dodecandioic acids, make peroxyacid bleach wet pulp body.
Step B
With the dried fine powder of DPDA of recirculation and sodium sulfate in shown in ratio fusion and being incorporated in the Turbulizer mixing tank.Dryer feed solid temperature is about 18 ℃.The size of DPDA fine powder is below 250 microns, and the granularity of sodium sulfate is then between about 180 to 285 microns.From a bucket, measure wet pulp body (30 ℃), it is sprayed on the dryer feed solid ingredient in the Turbulizer mixing tank with air atomization nozzle.With now for the material collection of wet granular form and transfer in the Aeromatic moisture eliminator.The temperature of the wet granular that comes out from the Turbulizer mixing tank is about 30 ℃.
Step C
With wet grain drying, the dry bleach particle of crossing cools off in moisture eliminator.
Analyze density, granularity and the chemical ingredients of final bleach particle then.At experimental session speed, blade angle and the gap of Turbulizer mixing tank are regulated to obtain optimum size.Wet granular in moisture eliminator with about 65 ℃ dry air about 30 minutes is as cold as about 18 ℃ then.
The dried particulate feature of the peroxyacid bleach of example 1 is as follows: moisture is about 0.2%, the about 0.64 gram/cubic centimetre of density, DPDA content about 25%; Boric acid content is about 27%, sodium sulfate about 46%.Nearly 90% grain graininess is in about 250 microns to 1750 microns scope, and mean particle size is about 500 ± 75 microns.
The tensio-active agent slurry of example 1 and the composition of accessory constituent composition are as follows:
The component umber
LAS(linear alkylbenzene sulfonate 28% 34.26
Vitriol 22%, water 50%)
Pyridine dicarboxylic acid (DPA) 0.09
Phosphoric acid (H 3PO 4) 0.2
Tertiary sodium phosphate (TSPP) 0.11
Amount to 34.66
With three kinds of accessory constituents (DPA, H 3PO 4And TSPP) with the LAS slurry in shown in ratio be pre-mixed.Anhydrous sodium sulphate plays filler effect, also has the usefulness of second heat release control agent/heat absorber simultaneously.
Example 2
Use following component:
Peroxyacid bleach wet pulp body umber
Two peroxide dodecandioic acids (DPDA) 25.55%; 3.01
Water 46.5%; Boric acid 19.68%; Surfactivity
Agent slurry+accessory constituent 8.27%
The dryer feed solid
Anhydrous sodium sulphate 1.28
Boric acid powder 0.25
The dried fine powder of the DPDA of recirculation (250 microns) 5.46
Amount to 10.00
Used equipment is 8 inches Turbulizer mixing tanks of Bepex and 1 square metre of continuous fluidized bed moisture eliminator of Bepex.Method and apparatus is similar with example 1, only has been to use continuous fluidized bed moisture eliminator.
Steps A
Boric acid and tensio-active agent slurry+accessory constituent are added in the aqueous solution of two peroxide dodecandioic acids, make peroxyacid bleach wet pulp body (30 ℃).
Step B
From bucket, measure wet pulp body (30 ℃), it is sprayed on the dried solid ingredient in the Turbulizer mixing tank (room temperature) with air atomization nozzle.
Step C
Wet granular in the Turbulizer mixing tank is transported in the Bepex fluidized bed dryer continuously, and the dry air in two district of Bepex fluidized-bed is about 65 ℃, and the temperature of control dried particles during drying keeps below about 30 ℃.To the SYNTHETIC OPTICAL WHITNER of supply ambient air in the 3rd district of Bepex fluidized-bed with cooling drying.The dried particle water content of final SYNTHETIC OPTICAL WHITNER is about 0.3%, and density is about 0.61 gram/cubic centimetre, DPDA24%, and boric acid is about 28%, sodium sulfate about 42.5%.
Vitriol in the example 2 and boric acid solid are with the charging respectively of capacity feeder.The dried fine powder of recirculation SYNTHETIC OPTICAL WHITNER that produces in fluidized bed dryer (step C) is recycled to after opening with the particle separation of want granularity in the mixing tank of step B and uses as the dryer feed solid.From moisture eliminator, remove granularity continuously less than about 250 microns bleach particle.Granularity is sifted out greater than the dried particle of about 1750 microns SYNTHETIC OPTICAL WHITNER, be ground to, and then circulation is as the dried fine powder use of solid of dryer feed among the step B less than about 250 microns.
In the continuous fluidized bed drying step of example 2 or 3, recirculation peroxyacid bleach fine powder in fluidized-bed in the adding previous round or the bleach particle that ground are as crystal seed.Fine powder, particle and other SYNTHETIC OPTICAL WHITNER as crystal seed are done solid ingredient, and its granularity is preferably less than 250 microns.When beginning this process preferably with the granular boric acid of formula rate and vitriol as dryer feed, dryer feed is mixed mutually with the peroxy acid slurry.First bleach particle gives off back recirculation by moisture eliminator and uses, until the material balance that reaches regulation.The temperature of dry air is about 60 ℃ to 70 ℃.
Example 3
Component utilized is as follows in this example:
Peroxyacid bleach wet pulp body umber
Two peroxide dodecandioic acids 28.6%; Water 52.2%; 2.99
Boric acid 11%; Tensio-active agent slurry+less important
Component 8.2%
The dryer feed solid
Anhydrous sodium sulphate 1.52
Boric acid powder 0.61
Lift the dried fine powder 6.88 of circulation DPDA again
Amount to 12.00
Equipment used is 8 inches Turbrlizer mixing tanks of Bepex and 3 square metres of continuous fluidized bed moisture eliminators of Bepex.
Steps A
Boric acid and tensio-active agent slurry+accessory constituent are added in the aqueous solution of two peroxide dodecandioic acids, make peroxyacid bleach wet pulp body.The temperature of wet pulp body is about 30 ℃.
Step B
From bucket, measure the wet pulp body, it is sprayed on the dryer feed solid in the Turbulizer mixing tank with the air atomizing nozzle.
The capacity feeder charging respectively of anhydrous sodium sulphate and boric acid solid.Particle separation with the dried fine powder of DPDA that produces in the fluidized bed dryer and the granularity of wanting is recycled in the Turbulizer mixing tank and uses as the dryer feed solid.
Step C
Wet granular in the Turbulizer mixing tank is transported in the fluidized bed dryer continuously, and the temperature of dry air is as follows:
70 ℃ in the 1st district
55 ℃ in the 2nd district
50 ℃ in the 3rd district
10 ℃ in the 4th district
The residence time of institute's exsiccant bleach particle in moisture eliminator is about 30 minutes.The temperature of SYNTHETIC OPTICAL WHITNER dry granular is about 22 ℃ when leaving moisture eliminator.Their free water content is about 0.3%.Density is about 0.63 gram/cubic centimetre, and DPDA content is about 26%, and boric acid content is about 28.4%, and it is about 42.5% that sodium sulphate content is about, and mean particle size is about 500 microns.
Productive rate in the example 3 is about 34% by dry.
Concentration as the peroxy acid of index among the example 3A is about 10%(vitriol as the thinner of doing by dry).Productive rate is about 81.9%(by dry and sees Table 1, example 3A).
Concentration as the peroxy acid of index among the example 3B is about 24% by dry.The moisture content of peroxy acid slurry is 32%.Productive rate is counted 78.95%(by dry and is seen Table 1, example 3B).
Table 1
Component example 3 example 3A example 3B
Umber umber umber
Peroxy acid slurry 2.99 2.99 4.87
(moisture % in the slurry) (52.2) (52.2) (32)
Anhydrous sodium sulphate 1.52 6.51 3.52
Boric acid 0.61 0.61 1.41
Recirculation fine powder/screening reject * 6.88 1.89 2.20
Amount to: 12.00 12.00 12.00
Dry output umber 10.44 10.44 10.44
Productive rate (by dry) 34.1% 81.9% 78.95%
Peroxy acid % 24 10 24
* drying process produces fine powder/screening reject recycled matter of 15% to 25% usually during balance.
A kind of recirculation DPDA fine powder composition that is suitable for example 1,2 and 3 is:
Two peroxide dodecandioic acids (DPDA) 24%
Sodium sulfate 43%
Boric acid 26%
LAS slurry 5.2%
Accessory constituent (comprises the Na in the slurry 2SO 4) 1.3%
Free water content 0.5%
Example 2 and 3 tensio-active agent slurry and accessory constituent composition are as follows:
The composition umber
LAS(linear alkylbenzene sulfonate 50%; 19.58
Vitriol 1%; Water 49%)
Pyridine dicarboxylic acid (DPA) 0.09
Phosphoric acid (H 3PO 4) 0.2
Tertiary sodium phosphate (TSPP) 0.11
Amount to 19.98
Three kinds of accessory constituents (DPA, H 3PO 4And TSPP) and LAS slurry in shown in ratio be pre-mixed.In prescription, add DPA, TSPP and H 3PO 4Be as sequestrant constraint heavy metal ion.LAS is used as processing aid.In all examples among the step C temperature of wet granular estimate all to be lower than about 30 ℃.
When successive processes of the present invention reached balance, the productive rate that comes out from moisture eliminator was about 75% to 85%.About 5% to 10% is screening reject, it is worn into the recirculation of DPDA fine powder use.Nearly 10% to 15% wet granular breaks away from moisture eliminator with fine powder form through degassing bag filter gathering system.

Claims (14)

1, a kind of dried granular bleaching agent product, it is made of the compound reunion mixture of peroxyacid bleach and peroxyacid bleach heat release control agent, and the quantity of heat release control agent is to play stabilization; The preparation method of wherein said dry granular shape SYNTHETIC OPTICAL WHITNER is as follows:
(I) be mechanically mixing following (A), (B) material continuously:
(A) but the peroxyacid bleach hygroscopicity slurry logistics of pump pound; This slurry contains about water of 26% to 55%, and is at least about 1/3rd the above-mentioned heat release control agent that can play stabilization quantity;
(B) particulate solid dryer feed, it is selected from the dried fine powder of SYNTHETIC OPTICAL WHITNER and atomizing heat release control agent salt, filler and their mixture of recirculation; Form the SYNTHETIC OPTICAL WHITNER wet granular that contains moisture by it, its free water content is about 10% to 20%;
The logistics of hygroscopicity slurry is pumped into above-mentionedly driedly to advance on the grain;
(II) is lower than above-mentioned SYNTHETIC OPTICAL WHITNER wet grain drying to free water content about 0.5% under controlled temperature in fluidized bed dryer, to obtain described dry granular shape SYNTHETIC OPTICAL WHITNER product.
2, the dry granular shape SYNTHETIC OPTICAL WHITNER product of claim 1 is characterized in that heat release control agent wherein is selected from following material: boric acid, oxysuccinic acid, toxilic acid, sodium sulfate, bitter salt, Magnesium Formate Dihydrate, calcium sulfate (CaSO 42H 2O), hydration calcium lactate, calcium sulfate sodium (CaSO 42Na 2SO 42H 2And aluminium sodium sulfate, potassium aluminium sulfate, exsiccated ammonium alum, the hydrate of this class material of Tai-Ace S 150 and its mixture O).
3, the dry granular shape SYNTHETIC OPTICAL WHITNER product of claim 1 is characterized in that, the content of heat release control agent wherein is about 70% to 400% of peroxyacid bleach weight.
4, the dry granular shape SYNTHETIC OPTICAL WHITNER product of claim 3 is characterized in that, it is about 0.5% that the water-content of bleach particle wherein is lower than, and density is at least about 0.5 gram/cubic centimetre, and the content of heat release control agent is about 75% to 200% of SYNTHETIC OPTICAL WHITNER weight.
5, the dry granular shape SYNTHETIC OPTICAL WHITNER product of claim 4 is characterized in that pellet density wherein is about 0.6 to 0.7 gram/cubic centimetre, and the content of heat release control agent is about 100% to 150% of SYNTHETIC OPTICAL WHITNER weight.
6, the dry granular shape SYNTHETIC OPTICAL WHITNER product of claim 1 is characterized in that heat release control agent wherein is selected from boric acid, toxilic acid, oxysuccinic acid, sodium sulfate, and their mixture.
7, the dry granular shape peroxyacid bleach product of claim 1 is characterized in that heat release control agent wherein is the mixture of sodium sulfate and boric acid, and the ratio of the two is about 1: 1 to 6: 1, and the content of boric acid is at least about 70% of peroxyacid bleach weight.
8, the method for the dry granular shape peroxyacid bleach product of preparation claim 1, it may further comprise the steps:
A. form hygroscopicity peroxyacid bleach slurry, it contains:
(1) about water of 26% to 55%;
(2) about peroxyacid bleach of 20% to 45%;
The heat release control agent of (3) 1/3 stabilization quantity;
B. the pumpable hygroscopicity slurry with steps A sprays on the dryer feed of the dried solid ingredient of SYNTHETIC OPTICAL WHITNER, forms the wet granular that contains 10-20% moisture;
C. with above-mentioned wet granular with about 35 ℃ to 100 ℃ air blast dry air.
9, the method for claim 8 is characterized in that, the water content of hygroscopicity slurry wherein is about 30% to 40%, and the water-content of wet granular is about 12% to 18%, and the final water content of particulate is about 0.1% to 0.3%.
10, the method for claim 8 is characterized in that, wherein the temperature of slurry is about 30 ℃ to the highest about 40 ℃, and fluidized-bed temperature is about 38 ℃ to 81 ℃, and the drying temperature of wet granular among the controlled step C makes it be lower than about 60 ℃ simultaneously.
11, the method for claim 8 is characterized in that, wherein the temperature of slurry is about 34 ℃ to the highest about 38 ℃, and fluidized-bed air blast air themperature is about 60 ℃ to 70 ℃.
12, the method for claim 8 is characterized in that, the content of peroxyacid bleach is about 10% to 35% in the dried particle wherein.
13, the method for claim 12 is characterized in that, the content of peroxyacid bleach wherein is about 20% to 30%.
14, the method for claim 8 is characterized in that, is about 0.2 second to 5 seconds in order to the mixing residence time that forms wet granular among the step B, is about 10 minutes to 60 minutes the time of drying among the step C.
CN 90102598 1989-05-01 1990-05-01 Agglomerated granular peroxyacid bleach and process for its preparation Pending CN1046932A (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US34549589A 1989-05-01 1989-05-01
US345,495 1989-05-01

Publications (1)

Publication Number Publication Date
CN1046932A true CN1046932A (en) 1990-11-14

Family

ID=23355289

Family Applications (1)

Application Number Title Priority Date Filing Date
CN 90102598 Pending CN1046932A (en) 1989-05-01 1990-05-01 Agglomerated granular peroxyacid bleach and process for its preparation

Country Status (8)

Country Link
EP (1) EP0396341A3 (en)
JP (1) JPH03800A (en)
CN (1) CN1046932A (en)
AU (1) AU643206B2 (en)
BR (1) BR9002050A (en)
CA (1) CA2015490A1 (en)
MA (1) MA21830A1 (en)
MX (1) MX173060B (en)

Families Citing this family (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AU666249B2 (en) * 1992-12-23 1996-02-01 Huntsman Surfactants Technology Corporation Granulation process
NZ258826A (en) * 1992-12-23 1996-12-20 Ici Australia Operations Granulation process for powdered detergent
EP0987315A1 (en) * 1998-09-16 2000-03-22 The Procter & Gamble Company Bleaching compositions
KR100593529B1 (en) 2004-03-31 2006-06-28 주식회사 엘지생활건강 Process for preparing ester type bleach activator compound
US12203056B2 (en) 2008-03-28 2025-01-21 Ecolab Usa Inc. Sulfoperoxycarboxylic acids, their preparation and methods of use as bleaching and antimicrobial agents
US8871807B2 (en) 2008-03-28 2014-10-28 Ecolab Usa Inc. Detergents capable of cleaning, bleaching, sanitizing and/or disinfecting textiles including sulfoperoxycarboxylic acids
US8809392B2 (en) 2008-03-28 2014-08-19 Ecolab Usa Inc. Sulfoperoxycarboxylic acids, their preparation and methods of use as bleaching and antimicrobial agents
MX2010010236A (en) 2008-03-28 2010-10-20 Ecolab Inc Sulfoperoxycarboxylic acids, their preparation and methods of use as bleaching and antimicrobial agents.
US9321664B2 (en) 2011-12-20 2016-04-26 Ecolab Usa Inc. Stable percarboxylic acid compositions and uses thereof
US9242879B2 (en) 2012-03-30 2016-01-26 Ecolab Usa Inc. Use of peracetic acid/hydrogen peroxide and peroxide-reducing agents for treatment of drilling fluids, frac fluids, flowback water and disposal water
US10165774B2 (en) 2013-03-05 2019-01-01 Ecolab Usa Inc. Defoamer useful in a peracid composition with anionic surfactants
US20140256811A1 (en) 2013-03-05 2014-09-11 Ecolab Usa Inc. Efficient stabilizer in controlling self accelerated decomposition temperature of peroxycarboxylic acid compositions with mineral acids
US8822719B1 (en) 2013-03-05 2014-09-02 Ecolab Usa Inc. Peroxycarboxylic acid compositions suitable for inline optical or conductivity monitoring
EP3841059A1 (en) 2018-08-22 2021-06-30 Ecolab USA Inc. Hydrogen peroxide and peracid stabilization with molecules based on a pyridine carboxylic acid at c-3, -4 or -5
US12096768B2 (en) 2019-08-07 2024-09-24 Ecolab Usa Inc. Polymeric and solid-supported chelators for stabilization of peracid-containing compositions

Family Cites Families (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3770816A (en) * 1969-07-23 1973-11-06 Ppg Industries Inc Diperisophthalic acid compositions
US4100095A (en) * 1976-08-27 1978-07-11 The Procter & Gamble Company Peroxyacid bleach composition having improved exotherm control
US4091544A (en) * 1977-02-11 1978-05-30 The Procter & Gamble Company Drying process
US4170453A (en) * 1977-06-03 1979-10-09 The Procter & Gamble Company Peroxyacid bleach composition
US4244884A (en) * 1979-07-12 1981-01-13 The Procter & Gamble Company Continuous process for making peroxycarboxylic acids
US4314949A (en) * 1980-07-23 1982-02-09 The Procter & Gamble Company Process for making peroxycarboxylic acids
US4497757A (en) * 1983-01-31 1985-02-05 The Procter & Gamble Company Energy efficient hydration process
DE3515712A1 (en) * 1985-05-02 1986-11-06 Henkel KGaA, 4000 Düsseldorf FLEACH, ITS PRODUCTION AND USE
EP0206418B1 (en) * 1985-06-28 1991-11-13 The Procter & Gamble Company Dry bleach and stable enzyme granular composition
GB8810630D0 (en) * 1988-05-05 1988-06-08 Unilever Plc Process for preparing bodies containing peroxyacid & compositions comprising said bodies
DE3822798A1 (en) * 1988-07-06 1990-01-11 Huels Chemische Werke Ag METHOD FOR THE PRODUCTION OF PHLEGMATIZED ALIPHATIC DIPEROXIDICARBONE ACIDS
US4917811A (en) * 1988-09-20 1990-04-17 Lever Brothers Company Bleach compositions and process for making same

Also Published As

Publication number Publication date
MX173060B (en) 1994-01-31
AU5454990A (en) 1990-11-01
MA21830A1 (en) 1990-12-31
EP0396341A2 (en) 1990-11-07
EP0396341A3 (en) 1992-01-22
CA2015490A1 (en) 1990-11-01
BR9002050A (en) 1991-08-13
AU643206B2 (en) 1993-11-11
JPH03800A (en) 1991-01-07

Similar Documents

Publication Publication Date Title
CN1046932A (en) Agglomerated granular peroxyacid bleach and process for its preparation
CN1030468C (en) Stable bleach-containing liquid detergent compositions
CN1146524C (en) Process for the preparation of sodium percarbonate and dry granular sodium percarbonate
CN1114686C (en) Stable solid block metal protecting warewashing detergent composition
CN1045311C (en) Detergent compositions
CN1026496C (en) Process for the preparation of detergents containing color-stable bleach activator extrudate particles
CN1105178C (en) Method for producing nonoionic detergent granules
CN1167782C (en) Granular detergent components and particulate detergent compositions containing them
CN1131300C (en) Free-flowing particulate detergent compsns.
CN1156563C (en) Process for making detergent composition by non-tower process
JPS6222899A (en) Bleaching activating additive, its production and detergent composition containing said additive
CN1187435C (en) Process for producing particulate washing or cleaning agent
CN1027286C (en) Granular bleach containing amido peroxyacids
CN1195839C (en) Particulate laundry detergent compositions containing anionic surfactant granules
CN1075332A (en) In the sulfonic acid and make the method for granulated detergent
CN1065565C (en) Process for preparing detergent compositions
CN1234825A (en) Agglomeration process for producing detergent compositions involving premixing modified polyamine polymers
CN1083859A (en) detergent composition
CN1077486A (en) High active detergent pastes
CN1120231C (en) Spray drying method for producing detergent composition involving premixing modified polyamine
CN1590524A (en) Process for producing granular anionic surfactant
CN1753981A (en) Anionic surfactant powder
EP0139539B1 (en) Process for the manufacture of detergent powder
JP2608238B2 (en) Stable sodium percarbonate, method for producing the same, and bleaching detergent composition containing stable sodium percarbonate
CN1233275A (en) Free-flowing agglomerated nonionic surfactant detergent composition and process for making same

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C01 Deemed withdrawal of patent application (patent law 1993)
WD01 Invention patent application deemed withdrawn after publication