CN100526213C - Preparation method for powdery sodium percarbonate - Google Patents
Preparation method for powdery sodium percarbonate Download PDFInfo
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- CN100526213C CN100526213C CNB2006100333170A CN200610033317A CN100526213C CN 100526213 C CN100526213 C CN 100526213C CN B2006100333170 A CNB2006100333170 A CN B2006100333170A CN 200610033317 A CN200610033317 A CN 200610033317A CN 100526213 C CN100526213 C CN 100526213C
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Abstract
The invention relates to a preparation method for the powder sodium percarbonate with active oxygen content at least 10% and 13. 5~15. 2% as the preferred value, which comprises: (A) mixing the anhydrous Na2CO3 and water with some proportion; (B) spraying the H2O2 solution with preferred quantity into the mixture obtained in (A) to make the Na2CO3 and H2O2 reaction fully at 0~70Deg and obtain the slurry of sodium percarbonate; (C) drying with rotation flash evaporation device to obtain the final product. This product is convenient to mix with other constituent, such as detergent and bleacher.
Description
Technical field
The invention belongs to the preparing technical field of peracid salt in the inorganic chemistry, the massfraction that relates in particular to a kind of active oxygen is the preparation method of 10% powdery sodium percarbonate (sodium percarbonate abbreviates PCS as) at least.
Background technology
SPC-D is a kind of performance gentleness, multi-functional SYNTHETIC OPTICAL WHITNER and washing auxiliary detergent, and total molecular formula is 2Na
2CO
33H
2O
2, the massfraction of theoretical active oxygen is 15.28% (to be equivalent to 32.49%H
2O
2).Discharge hydrogen peroxide and yellow soda ash after SPC-D is water-soluble, hydrogen peroxide produces a large amount of active oxygens under alkaline condition, have the stronger functions such as stain, bleaching, sterilization of going, and yellow soda ash is the washing auxiliary detergent of using always, therefore, SPC-D can be removed common stains such as milk stain, bloodstain, sweat stain, sebum, coffee stain, bloodstain and fruit syrup effectively.The main component that SPC-D both can be used as household bleach and removed stain cleanser, also can be used as washing auxiliary detergent, add to phosphorous or non-phosphide detergent in, or as the bleaching component of dish washing compositions and hard-surface cleaning composition, strengthen and go to steep function, improve washing effect.Also can be used as disinfection sanitizer, oxygenate, cleaning agent for mouth cavity and waste water conditioner.The characteristics of SPC-D are good water solubility, and the performance gentleness can not damaged fabric fibre and color, and the generation that has no irritating odor, and degradation production can not increase carrying capacity of environment.
SPC-D generally adopts yellow soda ash and aqueous hydrogen peroxide solution reaction to obtain, and discloses three kinds of processing methodes in the prior art: crystallization process, fluidized bed process and dry method.
Crystallization process be aqueous sodium carbonate and aqueous hydrogen peroxide solution 0～20 ℃ of reaction down, separate out sodium percarbonate crystal, after filtration or centrifugation, fluidised bed drying, then granular SPC-D.In order to separate out sodium percarbonate crystal as much as possible, in reaction process, often add salting-out agent such as sodium-chlor.Crystallization process is realized the mixing between the material easily, heat can in time be removed, easy control of temperature, product stability is good, but complex process, facility investment is big, contain more unreacted hydrogen peroxide in the mother liquor, ability reuse after needing to decompose has increased production cost, and have partial mother liquid to need discharging, cause environmental pollution.The SPC-D that crystallization process obtains has many purposes, but is not best, and the salt of adding also can influence its application.Size of particles and bulk density are wayward, and the particle dissolution rate is slow, and some occasion is used inconvenience.
Fluidized bed process is that aqueous hydrogen peroxide solution and sodium carbonate solution are continuously sprayed in the fluidized-bed that contains the small nucleus of SPC-D respectively or after the moment mixing according to a certain percentage, utilize warm air to take away moisture, product obtains the granulous SPC-D after cooling.The product granularity of this method gained is even, and raw material consumption is lower, and device is compact, is particularly suitable for continuous mass production, and reaction heat can in time be removed.But need remove a large amount of moisture, energy expenditure is higher; Nozzle stops up easily, and the operational requirement strictness is wayward.
Dry method is with the solid anhydrous sodium carbonate or hydrated sodium carbonate is direct and the aqueous hydrogen peroxide solution reaction, and technology is simple, and facility investment is few, hydrogen peroxide utilization ratio height, and production cost is lower.Because the heat transfer efficiency between the solid is not as liquid, the key that realizes dry method is exactly will react the heat that produces effectively in time to derive.If do not mix efficiently and heat passage heat is in time removed, temperature can raise fast, causes hydrogen peroxide and SPC-D to decompose, and decomposes can produce a large amount of heats again, and further accelerate decomposition finally causes operating out of control.
Dry method is divided into a step dry method and two step dry method, and a step dry method is that anhydrous sodium carbonate mixes with aqueous hydrogen peroxide solution under violent stirring, and reaction generates SPC-D rapidly.U.S. Pat 5045296 and US5328721 disclosed method are with 65%～85% aqueous hydrogen peroxide solution and anhydrous sodium carbonate reaction, when adding superoxol in the reactor bubbling air, keeping temperature of reaction is 50～80 ℃, the vaporization free-water.The size distribution of SPC-D product is identical with the yellow soda ash raw material, and active o content is 13.0%～14.5%.
Two step method is earlier anhydrous sodium carbonate to be mixed with water, is modulated into monohydrated sodium carbonate or contains the yellow soda ash of free-water, and then react with aqueous hydrogen peroxide solution and obtain SPC-D, solves the heat transfer problem of process preferably.For example Chinese patent application CN1240407A disclosed method is; be modulated into monohydrated sodium carbonate by anhydrous sodium carbonate; react with aqueous hydrogen peroxide solution again; drying obtains unbodied SPC-D primary granule; repressed, granulation, and then obtain sodium percarbonate granules, active o content is 14.5%～15.2%; median size is 550～1100 μ m, and tap density is 0.93～1.1g/cm
3Monohydrated sodium carbonate is with the water-bath preheating of anhydrous sodium carbonate with 99 ℃, and the boiled water with 1.0～1.5 times of molar weights obtains at the time enough internal reaction again.
U.S. Patent application US2004/0161378A1 disclosed method is, mixes with water at 15～30 ℃ of following anhydrous sodium carbonates, obtains water-content and be 5%～10% agglomerate, and water is to exist with free form, rather than exists with the form of hydrate.The spray aqueous hydrogen peroxide solution is blown into air simultaneously, 20～80 ℃ of control reaction temperature, and the moisture of reaction mixture maintains 5%～20%.Fluidised bed drying obtains the sodium percarbonate granules of active o content 14.0%～14.9%, particle diameter 500～800 μ m, bulk density 0.90～1.05g/cm
3
In prior preparation method, use conventional stablizers such as silicate, magnesium salts, the SPC-D of gained absorbs airborne moisture easily and causes decomposing, therefore, existing method is prepared into SPC-D the granulous solid usually, and bulk density and particle size generally seldom are variable, in most of the cases, at the very start it is limited in the narrower scope by processing method or employed yellow soda ash.
According to the difference of end-use, household chemicals manufacturers needs different SPC-D, and what for example add in washing powder is the granulous SPC-D, then adds the powdered SPC-D in cleaning agent for mouth cavity, toothpaste, makeup.If the particle of the bulk density of SPC-D, granular size and washing powder, sanitising agent or whitener composition is not in tune, just be difficult to mix, even mix, in packing, transportation and storage process, also can produce segregation, cause each component skewness in product, influence result of use.After other composition of compositions such as powdery sodium percarbonate and washing composition, SYNTHETIC OPTICAL WHITNER or sanitising agent mixes, granulation again, no matter when product all is uniformly, has guaranteed result of use.Some components of washing composition, sanitising agent or SYNTHETIC OPTICAL WHITNER only have its aqueous solution supply on market, because SPC-D can't directly be added in washing composition, sanitising agent or the SYNTHETIC OPTICAL WHITNER that contains SPC-D the susceptibility of water.And other components can buy powdery or granular product, but price is much more expensive than its aqua, and this has increased the production cost of washing composition, sanitising agent or SYNTHETIC OPTICAL WHITNER undoubtedly.After the aqueous solution short mix of powdery sodium percarbonate and these compositions, granulating and drying just can make required washing composition, sanitising agent or whitener composition easily again.According to different purposes, the content of SPC-D can be regulated arbitrarily, and can make and vary in size, and is different, washing composition, sanitising agent or SYNTHETIC OPTICAL WHITNER that release rate is different.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of preparation method of powdery sodium percarbonate, and the powdery sodium percarbonate of gained can be used for some inconvenience maybe can not use compositions such as the washing composition of granular sodium percarbonate, sanitising agent, SYNTHETIC OPTICAL WHITNER.According to different cleaning tasks, the consumption that can regulate SPC-D in these compositions easily satisfies the needs of its function.Method of the present invention need not to control in the mixing process of anhydrous sodium carbonate and water and must form monohydrated sodium carbonate, or makes water form agglomerate with free form and yellow soda ash.The dry method that the present invention proposes can provide the high quality SPC-D especially under high as far as possible active oxygen productive rate, according to different application targets, the active oxygen massfraction in the SPC-D that provides is variable.
The massfraction that the invention provides a kind of active oxygen is preparation method's (dry method) of 10% powdery sodium percarbonate at least, and its feature follows these steps to carry out:
(A) anhydrous sodium carbonate and water are by a certain percentage: the mol ratio of water and yellow soda ash is 0.5:1 to＜1:1, mixes, and obtains the mixture of yellow soda ash, water;
(B) aqueous hydrogen peroxide solution is sprayed in the mixture of (A) step gained, the amount of hydrogen peroxide adds according to the accurate stoichiometric quantity of desirable active o content in the SPC-D, the whole spray time of aqueous hydrogen peroxide solution is equally divided into leading portion and back segment, the spray rate of control leading portion aqueous hydrogen peroxide solution is 1/2 of a back segment spray rate, yellow soda ash and hydrogen peroxide are fully reacted, control reaction temperature is in 0～70 ℃ scope, superoxol has sprayed the back and has continued reaction 3～10 minutes, obtains the slurry or the mashed prod of SPC-D;
(C) take out product, and enter Rotatingandflashstreamingdrier by screw feeder and carry out drying, the massfraction that obtains active oxygen is 10%～15.2% powdery sodium percarbonate.
Described anhydrous sodium carbonate is light sodium carbonate or heavy yellow soda ash or their mixture.
The mol ratio of described water and yellow soda ash, preferred mol ratio are 0.8:1 to＜1:1.
Except containing yellow soda ash and water, contain a kind of in monohydrated sodium carbonate, sodium carbonate heptahydrate and the Sodium carbonate decahydrate at least in the mixture of described anhydrous sodium carbonate and water mixing gained.
The described temperature of reaction that keeps in the reaction process of yellow soda ash, water mixture and hydrogen peroxide is in 0～70 ℃ scope.
Described in the reaction process of yellow soda ash, water mixture and hydrogen peroxide temperature of reaction preferably be controlled in 15～40 ℃ the scope.
The method of the preparation of described powdery sodium percarbonate is 2Na with theoretical molecular formula
2CO
33H
2O
2SPC-D be the benchmark meter, use the aqueous hydrogen peroxide solution of accurate stoichiometric quantity, add 1.49～1.52 moles aqueous hydrogen peroxide solution in every mole of yellow soda ash.
The concentration of described aqueous hydrogen peroxide solution is 27.5%～70%.
The concentration of described aqueous hydrogen peroxide solution is preferably 35%～50%.
The adding massfraction is 50%～60% 1-hydroxyl ethane-1 in the described aqueous hydrogen peroxide solution, 1-Disodium alendronate solution.
The method of the preparation of described powdery sodium percarbonate, 1-hydroxyl ethane-1, the add-on of 1-Disodium alendronate is 2%～10% of a hydrogen peroxide quality, is preferably 3%～7%.
The method of the preparation of described powdery sodium percarbonate, yellow soda ash, water mixture add reactor in batches in periodical operation technology, react with the hydrogen peroxide that sprays into, and have sprayed the back and have continued reaction 3～10 minutes.
The method of the preparation of described powdery sodium percarbonate, the temperature of inlet air was selected in 110～180 ℃ when Rotatingandflashstreamingdrier was dry.
The method of the preparation of described powdery sodium percarbonate, the temperature of inlet air was preferably 140～180 ℃ when Rotatingandflashstreamingdrier was dry; Outlet Gas Temperature is controlled in 50～70 ℃.
Method of the present invention can be used the anhydrous sodium carbonate of all size that can obtain on the market, not influenced with the different of shape, density by the size of yellow soda ash kind, preparation method, particle.Density is 500～600kg/m
3Light sodium carbonate, density is 1000～1200kg/m
3Heavy yellow soda ash, density is 370kg/m
3Ultralight matter yellow soda ash, density is 1550～2553kg/m
3Overweight matter yellow soda ash, or their mixture all can be used for the present invention.Preferred light sodium carbonate, because its low price not only, in liberal supply, it is convenient to buy, and is easy to mix with water.
Preparation yellow soda ash, the employed water of water mixture can be tap water, pure water, preferred pure water.There is water to have metal ions meeting catalytic decomposition hydrogen peroxide and SPC-D such as iron, manganese, copper down, if this type of metal ion content is too high in the water, yellow soda ash, water mixture with the reaction process of superoxol in can cause the decomposition of hydrogen peroxide and SPC-D, increase consumption, therefore belong to ionic content in order to control underwater gold, it is favourable selecting pure water.The mol ratio of water and yellow soda ash is 0.5:1 to＜1:1, and preferred mol ratio is 0.8:1 to＜1:1.The mode that water can adopt in batches or spray adds, and the speed that adds water is criterion to help that the anhydrous sodium carbonate and the water capacity easily mixes, and the temperature of control mixture is no more than 90 ℃, and the temperature of preferred mixture is no more than 80 ℃.
Yellow soda ash can carry out in any equipment that both are mixed with mixing of water, both can intermittently carry out, and also can carry out continuously.Common mixing equipment, as ribbon mixer, colter formula mixing machine, moment weightless mix particles equipment, the planet cone-type mixer all can be used for the present invention.Have the screw extrusion press of pinch function, the mixing that kneader also can be used for both.
The mixing time of anhydrous sodium carbonate and water depends on the adding situation of handled amount, mixing equipment and water.Mix and generally in 10～60 minutes, finish.The length of mixing time is not strict, but strict control moisture is uniformly dispersed in the mixture of yellow soda ash, water.
The yellow soda ash, the water mixture that mix the back gained can directly react with superoxol, also behind available cycles water or the naturally cooling again with the superoxol reaction, react with superoxol again after preferably cooling off.At least contain a kind of in monohydrated sodium carbonate, sodium carbonate heptahydrate and the Sodium carbonate decahydrate in yellow soda ash, the water mixture, needn't strict control content separately.
The concentration of aqueous hydrogen peroxide solution of the present invention can be selected between 27.5%～70%, and preferred concentration is 35%～50%.General stable peroxide hydrogen in a manner known way, all known active oxygen stablizers all are fit in the prior art, for example 1-hydroxyl ethane-1,1-di 2 ethylhexyl phosphonic acid or its sodium salt.1-hydroxyl ethane-1, the concentration of 1-Disodium alendronate is generally 50%～60% (quality), with hydrogen peroxide (100%) is benchmark, 1-hydroxyl ethane-1, the consumption of 1-Disodium alendronate (100%) is 2%～10% (quality), be preferably 3%～7% (quality), be added in the aqueous hydrogen peroxide solution and mix, be made into mixed solution of hydrogen peroxide.
The mol ratio of yellow soda ash and hydrogen peroxide can be regulated the requirement of active o content according to the SPC-D end-use, in the method for the invention, yellow soda ash and hydrogen peroxide mol ratio obtain the content of active oxygen corresponding to desire in the SPC-D, wherein only require excessive slightly hydrogen peroxide if desired, be up to about 5% as the excessive order of magnitude.Because method of the present invention has guaranteed to react basically active oxygen productive rate completely, so use the hydrogen peroxide of accurate stoichiometric quantity (to be 2Na with respect to the total molecular formula of theory
2CO
33H
2O
2SPC-D, the massfraction of theoretical active oxygen is 15.28%) enough, and avoid making expensive hydrogen peroxide excessive in a large number.The mol ratio of hydrogen peroxide and yellow soda ash is about at 1.0 o'clock, and the massfraction that obtains active oxygen is about 10% SPC-D.In the preferred embodiment of the invention, the mol ratio of hydrogen peroxide and yellow soda ash is adjusted to about 1.49:1～1.52:1, so that the massfraction of active oxygen is 10% at least in SPC-D, be 13.5%～15.2% especially.
Can make yellow soda ash, water mixture and aqueous hydrogen peroxide solution fast enough and the violent various mixing tanks of blended can be used as the reactor of the inventive method.The reactor that is fit to is for example as follows: ribbon mixer, two rotors mixing machine, high speed intensive mixer, kneader.Preferred reactor is ribbon mixer and kneader, can be particularly well and handle slurry or the mashed prod that during reaction forms equably by means of kneader.When periodical operation, the yellow soda ash, the water mixture that prepare in advance can be put in the reactor, spray into superoxol at a certain temperature and react, reactor can be same reactor with preparation yellow soda ash, water mixture, also can be different reactors.Under andnon-continuous operation manner, preferably, aqueous hydrogen peroxide solution is metered in the reactor according to needed amount by nozzle.
In order to realize the thermopositive reaction between yellow soda ash and the aqueous hydrogen peroxide solution better, employed reactor equipment refrigerating unit comes control reaction temperature.Exempt from decomposition in order in time to remove reaction heat with protection hydrogen peroxide and SPC-D, this is particularly suitable.In order to cool off, can suitably cool off through a simple chuck, heat-eliminating medium can adopt recirculated cooling water or chilled water.In reaction process, temperature of reaction can be increased to 70 ℃ fully, and can not damage the performance, particularly active o content of product.But should avoid being higher than 70 ℃ temperature,, thereby influence the productive rate of product active oxygen because too high temperature can cause and quicken the decomposition of hydrogen peroxide and SPC-D.Reaction can be carried out being low to moderate under 0 ℃ the temperature, and can not influence product property, but should avoid being lower than 0 ℃ temperature, and slower because temperature is lower than the speed of response of 0 ℃ of hydrogen peroxide and yellow soda ash, the reaction times increases, and influences the throughput of device.Temperature control during reaction is without a doubt, and temperature of reaction advantageously remains in 0～70 ℃ the scope, and preferred temperature of reaction is 15～40 ℃.
The inventive method also should the strict spray rate of controlling superoxol except taking away the heat by recirculated cooling water in the cooling jacket or chilled water.By regulating the spray rate of hydrogen peroxide, make the quantity of heat production in the system unit time little in the fluctuation of entire reaction stage, help recirculated cooling water or chilled water and in time take away heat.Can change spray rate according to the variation of temperature of reaction.All reduce the decomposition of hydrogen peroxide and SPC-D with control reaction temperature, and the productive rate that has improved active oxygen is a prerequisite.The whole spray time of superoxol is equally divided into leading portion and back segment, and the spray rate of leading portion hydrogen peroxide is 1/2 of a back segment spray rate.
The speed of response of yellow soda ash and aqueous hydrogen peroxide solution is very fast, for periodical operation, reaction times is depended on the amount of desire reaction and the effect of heat exchange, as every batch of mixture that contains 500kg yellow soda ash, the spray of superoxol generally can be finished in the scope at 0.3～2 hour, particularly in 0.5～1 hour.Superoxol has sprayed back continuation reaction and had got final product in 3～10 minutes.
Except adding 1-hydroxyl ethane-1, beyond 1-di 2 ethylhexyl phosphonic acid or its sodium salt used as stabilizers, method of the present invention can optionally be added some other existing conventional stablizers or sequestrant comes stable peroxide hydrogen and SPC-D, silicate such as stablizer such as water glass, Starso, magnesium salts such as sal epsom, magnesium chloride, sequestrant such as sodium nitrilo triacetate (NTA), edetate (EDTA disodium or four sodium), amino trimethylene phosphonic salt (ATMP), ethylenediamine tetramethylene phosphonic acid salt (EDTMP).The adding mode of stablizer or sequestrant is varied, can be added in the aqueous hydrogen peroxide solution, or spray in the mixture of yellow soda ash, water, or be added in reaction process in the mixture of reaction.
The drying of the wet reaction product of pulpous state or pasty state is to carry out in Rotatingandflashstreamingdrier (also claiming the swirling eddy flash dryer, spin flash dryer).Select different big or small drying machines according to the output of powdery sodium percarbonate, the temperature in the kiln is generally in 80～120 ℃ scope.The temperature of inlet air can be selected in 110～180 ℃ according to different thermals source, makes thermal source as selecting steam, and the temperature of preferred inlet air is 140～180 ℃.Temperature out is selected to place one's entire reliance upon to the requirement of the final water content of product, with material properties also be closely bound up, to consider the temperature environment of discharging packing simultaneously.For fear of in cyclonic separator, separating out water of condensation, destroy operation, Outlet Gas Temperature should be strict controlled in 50～70 ℃.
When Rotatingandflashstreamingdrier was dry, the warm air tangent line entered the moisture eliminator bottom, formed strong rotation wind field under agitator drives.The reaction product wet feed is entered in the moisture eliminator by screw feeder, under the strong effect of high speed rotating stirring rake, material is impacted, obtain disperseing under the effect of friction and shearing force, lumpy material is pulverized rapidly, fully contacts with warm air, is heated, the dry material after dry, the dehydration rises with hot gas flow, collect product by cyclonic separator, fly-ash separator recovery dust does not parch or oversize material is got rid of to wall by centrifugal action, falls the bottom again and is pulverized dry.
The SPC-D of gained of the present invention is a powdery sodium percarbonate, and the content of its active oxygen is higher, is 10% (quality) at least, particularly 13.5%～15.2% (quality).In the time of in being combined to compositions such as washing composition, sanitising agent or SYNTHETIC OPTICAL WHITNER, the SPC-D of adding same amount then can obtain the higher product of active o content.Powdery sodium percarbonate of the present invention is stable, 105 ℃ down 2 hours thermostabilitys of heating be 90% at least, particularly 94%～98%.Product loss of active oxygen in storage period is less, helps the preservation and the use of product.
The analytical procedure of SPC-D:
(1) mensuration of active o content
Measure according to the method among the standard HG/T2764-1996, concrete steps are: take by weighing about 0.2g sample (being accurate to 0.0002g), place Erlenmeyer flask, wetting with less water, adding the 100ml sulphuric acid soln all dissolves sample, shake up, to the solution pinkiness, and in 30s, do not disappear and be terminal point with the titration of potassium permanganate standard titration solution.Do blank test simultaneously.
(2) mensuration of moisture
Measure according to the method among the standard HG/T2764-1996, concrete steps are: take by weighing about 3g sample (being accurate to 0.1g), place the weighing bottle of constant mass, be dried to constant mass in 140 ℃ in baking oven.
(3) mensuration of thermostability
The SPC-D sample that takes by weighing 30g known activity oxygen level is in the 50ml porcelain crucible, sample surfaces is shaken flat,, be cooled to room temperature 105 ℃ of down heating 2 hours, take by weighing 0.2 left and right sides sample and measure its active o content, measuring method is measured with the SPC-D active o content.
Thermostability (%)=(active o content before test back active o content/test) * 100.
The present invention has following advantage and beneficial effect:
The invention provides a kind of homogeneous, stable, transformable powdery sodium percarbonate of active o content and simple and economic preparation method, its active o content is 10%～15.2% (quality), particularly 13.5%～15.2% (quality).Compare with crystallization process, method of the present invention is to save energy, and temperature of reaction can be higher, and the reaction times is shorter, is used for the required cold of control reaction temperature still less, even can comes controlled temperature with recirculated cooling water.The SPC-D of the inventive method preparation is chloride not, therefore can avoid the danger of equipment corrosion.Method of the present invention does not produce the waste water of need handling, and crystallization process alkalogenic, contain hydrogen peroxide and muriatic waste water.With the massfraction of some SPC-D active oxygen only is that about 10% so-called dry method is different, can obtain 10%～15.2% (quality) according to method of the present invention, particularly the variable active o content of 13.5%～15.2% (quality); And the range of choice of raw material yellow soda ash, hydrogen peroxide is wideer, and operation, control are easier.The present invention prepares the mixture of yellow soda ash and water, needn't control the formation monohydrated sodium carbonate, or water is existed with the free form, the entire reaction phase temperature fluctuation of mixture and superoxol is little, guarantee hydrogen peroxide almost free of losses in reaction process, and therefore guarantee basically active oxygen productive rate completely.Therefore can avoid the hydrogen peroxide of costliness excessive, and the reaction of yellow soda ash and hydrogen peroxide can be carried out according to accurate stoichiometry.Method of the present invention is very flexibly, can control active o content in the SPC-D product well according to the present invention, and the SPC-D of dry back gained is powdered, needn't pulverize again.In addition, the SPC-D according to the inventive method preparation has the homogeneity of height.The powdery sodium percarbonate of the inventive method gained can be used for some inconvenience maybe can not use compositions such as the washing composition of granular sodium percarbonate, sanitising agent, SYNTHETIC OPTICAL WHITNER.Can be easily and other combination of components, prepare washing composition, sanitising agent or the SYNTHETIC OPTICAL WHITNER of different activities oxygen level according to different needs, make it to adapt to various requirement and different products on the market.
Embodiment
The following examples are used to further describe the present invention, yet are not to limit the present invention in the scope of these embodiment.% in the literary composition all is expressed as quality %.
Embodiment 1
With the 300.0kg light sodium carbonate (with Na
2CO
3Meter 98.8%) is added to 1m
3In the ribbon mixer, start stirring, spray into the 50.0kg pure water, the temperature of control mixture is no more than 80 ℃, mixes.The cooling, obtain yellow soda ash, water mixture, wherein the content of yellow soda ash is 87.3%, and with this mixture transposition in 1.5m
3Kneader in.At 284.0kg (with H
2O
2Meter 50.2%) adding concentration in the aqueous hydrogen peroxide solution is 50.3% 1-hydroxyl ethane-1, and 1-Disodium alendronate solution 8.5kg stirs and is made into uniform mixed solution of hydrogen peroxide.Start the stirring of kneader, the mixed solution of hydrogen peroxide of being joined is sprayed in the kneader, spray time amounts to about 30 minutes.The spray rate of preceding 15 minutes hydrogen peroxide is 1/2 of back 15 minutes spray rates.For control reaction temperature, adopt recirculated cooling water to cool off through the kneader chuck, regulate the flow of recirculated cooling water, control reaction temperature is 65～70 ℃.Superoxol has sprayed the back and has continued reaction 5 minutes, takes out product then from kneader, and is entered by screw feeder and to carry out drying in the Rotatingandflashstreamingdrier, and inlet air temperature is 150 ℃, and Outlet Gas Temperature is about 60 ℃.Obtain the powdery sodium percarbonate product, active o content 14.30%, moisture content 0.8%, thermostability are 96.27%.
Embodiment 2
With 300.0kg heavy yellow soda ash (with Na
2CO
3Meter 98.9%) is added to 1m
3In the ribbon mixer, start stirring, spray into the 25.2kg pure water, controlled temperature is no more than 80 ℃, mixes.The cooling, obtain yellow soda ash, water mixture, wherein the content of yellow soda ash is 91.8%, and with this mixture transposition in 1.5m
3Kneader in.At 514.0kg (with H
2O
2Meter 27.8%) adding concentration in the aqueous hydrogen peroxide solution is 50.3% 1-hydroxyl ethane-1, and 1-Disodium alendronate solution 8.5kg stirs and is made into uniform mixed solution of hydrogen peroxide.Start the stirring of kneader, the mixed solution of hydrogen peroxide of being joined is sprayed in the kneader, spray time amounts to about 40 minutes.Preceding 20 minutes spray rate is 1/2 of back 20 minutes spray rates.For control reaction temperature, adopt about-10 ℃ chilled water to cool off through the kneader chuck, regulate the flow of chilled water, 0～5 ℃ of control reaction temperature.Superoxol has sprayed the back and has continued reaction 10 minutes, takes out product then from kneader, and is entered by screw feeder and to carry out drying in the Rotatingandflashstreamingdrier, and inlet air temperature is 180 ℃, and Outlet Gas Temperature is about 70 ℃.Obtain the powdery sodium percarbonate product, active o content 14.80%, moisture content 0.7%, thermostability are 95.38%.
Embodiment 3
With the 300.0kg light sodium carbonate (with Na
2CO
3Meter 98.8%) is added to 1m
3In the ribbon mixer, start stirring, spray into the 40.0kg pure water, controlled temperature is no more than 90 ℃, mixes.The cooling, obtain yellow soda ash, water mixture, wherein the content of yellow soda ash is 87.5%, and with this mixture transposition in 1.5m
3Kneader in.At 203.0kg (with H
2O
2Meter 70.3%) adding concentration in the aqueous hydrogen peroxide solution is 50.3% 1-hydroxyl ethane-1, and 1-Disodium alendronate solution 8.5kg stirs and is made into uniform mixed solution of hydrogen peroxide.Start the stirring of kneader, the mixed solution of hydrogen peroxide of being joined is sprayed in the kneader, spray time amounts to about 30 minutes.The spray rate of preceding 15 minutes hydrogen peroxide is 1/2 of back 15 minutes spray rates.For control reaction temperature, adopt-5 ℃ of left and right sides chilled waters to cool off through the kneader chuck, regulate the flow of chilled water, control reaction temperature is 35～40 ℃.Superoxol has sprayed the back and has continued reaction 3 minutes, takes out product then from kneader, and is entered by screw feeder and to carry out drying in the Rotatingandflashstreamingdrier, and inlet air temperature is 110 ℃, and Outlet Gas Temperature is about 50 ℃.Obtain the powdery sodium percarbonate product, active o content 15.18%, moisture content 0.8%, thermostability are 96.60%.
Embodiment 4
With the 300.0kg light sodium carbonate (with Na
2CO
3Meter 98.8%) is added to 1m
3In the ribbon mixer, start stirring, spray into the 50.0kg tap water, controlled temperature is no more than 90 ℃, mixes.The cooling, obtain yellow soda ash, water mixture, wherein the content of yellow soda ash is 85.3%, and with this mixture transposition in 1.5m
3Kneader in.At 190.0kg (with H
2O
2Meter 50.2%) adding concentration in the aqueous hydrogen peroxide solution is 50.3% 1-hydroxyl ethane-1, and 1-Disodium alendronate solution 3.8kg stirs and is made into uniform mixed solution of hydrogen peroxide.Start the stirring of kneader, the mixed solution of hydrogen peroxide of being joined is sprayed in the kneader, spray time amounts to about 30 minutes.The spray rate of preceding 15 minutes hydrogen peroxide is 1/2 of back 15 minutes spray rates.For control reaction temperature, adopt-5 ℃ of left and right sides chilled waters to cool off through the kneader chuck, regulate the flow of chilled water, control reaction temperature is 35～40 ℃.Superoxol has sprayed the back and has continued reaction 5 minutes, takes out product then from kneader, and is entered by screw feeder and to carry out drying in the Rotatingandflashstreamingdrier, and inlet air temperature is 150 ℃, and Outlet Gas Temperature is about 60 ℃.Obtain the powdery sodium percarbonate product, active o content 10.14%, moisture content 0.9%, thermostability are 90.50%.
Embodiment 5
With the 150.0kg light sodium carbonate (with Na
2CO
3The meter 98.8%) and 150.0kg heavy yellow soda ash (with Na
2CO
3Meter 98.9%) is added to 1m
3In the ribbon mixer, start stirring, spray into the 40.3kg pure water, mix.Be cooled to room temperature, obtain yellow soda ash, water mixture, wherein the content of yellow soda ash is 87.2%, and with this mixture transposition in 1.5m
3Kneader in.At 282.0kg (with H
2O
2Meter 50.2%) adding concentration in the aqueous hydrogen peroxide solution is 50.3% 1-hydroxyl ethane-1, and 1-Disodium alendronate solution 28.1kg stirs and is made into uniform mixed solution of hydrogen peroxide.Start the stirring of kneader, the mixed solution of hydrogen peroxide of being joined is sprayed in the kneader, spray time amounts to about 30 minutes.The spray rate of preceding 15 minutes hydrogen peroxide is 1/2 of back 15 minutes spray rates.For control reaction temperature, adopt-5 ℃ of left and right sides chilled waters to cool off through the kneader chuck, regulate the flow of chilled water, control reaction temperature is 35～40 ℃.Superoxol has sprayed the back and has continued reaction 5 minutes, takes out product then from kneader, and is entered by screw feeder and to carry out drying in the Rotatingandflashstreamingdrier, and inlet air temperature is about 150 ℃, and Outlet Gas Temperature is about 60 ℃.Obtain the powdery sodium percarbonate product, active o content 14.12%, moisture content 0.9%, thermostability are 98.05%.
Embodiment 6
With the 240.0kg light sodium carbonate (with Na
2CO
3Meter 98.8%) is added to 1m
3In the ribbon mixer, start stirring, spray into the 40.2kg pure water, controlled temperature is no more than 90 ℃, mixes.Cooling obtains yellow soda ash, water mixture, and wherein the content of yellow soda ash is 85.1%.At 326.4kg (with H
2O
2Meter 35.4%) adding concentration in the aqueous hydrogen peroxide solution is 50.3% 1-hydroxyl ethane-1, and 1-Disodium alendronate solution 11.4kg stirs and is made into uniform mixed solution of hydrogen peroxide.The mixed solution of hydrogen peroxide of being joined is sprayed in the ribbon mixer, and spray time adds up to 80 minutes.The spray rate of preceding 40 minutes hydrogen peroxide is 1/2 of back 40 minutes spray rates.For control reaction temperature, adopt-5 ℃ of left and right sides chilled waters to cool off through the mixing machine chuck, regulate the flow of chilled water, control reaction temperature is 35～40 ℃.Superoxol has sprayed the back and has continued reaction 10 minutes, takes out product then from mixing machine, and carries out drying with Rotatingandflashstreamingdrier, and inlet air temperature is about 150 ℃, and Outlet Gas Temperature is about 60 ℃.Obtain the powdered SPC-D, active o content 13.85%, moisture content 0.9%, thermostability are 94.09%.
Claims (9)
1. the massfraction of an active oxygen is the preparation method of 10% powdery sodium percarbonate at least, it is characterized in that this method follows these steps to carry out:
(A) anhydrous sodium carbonate and water are by a certain percentage: the mol ratio of water and yellow soda ash is 0.5:1 to＜1:1, mixes, and obtains the mixture of yellow soda ash, water;
(B) aqueous hydrogen peroxide solution is sprayed in the mixture of (A) step gained, the amount of hydrogen peroxide adds according to the accurate stoichiometric quantity of desirable active o content in the SPC-D, the whole spray time of aqueous hydrogen peroxide solution is equally divided into leading portion and back segment, the spray rate of control leading portion aqueous hydrogen peroxide solution is 1/2 of a back segment spray rate, yellow soda ash and hydrogen peroxide are fully reacted, control reaction temperature is in 0～70 ℃ scope, superoxol has sprayed the back and has continued reaction 3～10 minutes, obtains the slurry or the mashed prod of SPC-D;
(C) take out product, and enter Rotatingandflashstreamingdrier by screw feeder and carry out drying, the massfraction that obtains active oxygen is 10%～15.2% powdery sodium percarbonate.
2. the method for the preparation of powdery sodium percarbonate according to claim 1 is characterized in that, anhydrous sodium carbonate is light sodium carbonate or heavy yellow soda ash or their mixture.
3. the method for the preparation of powdery sodium percarbonate according to claim 1, it is characterized in that, except containing yellow soda ash and water, contain a kind of in monohydrated sodium carbonate, sodium carbonate heptahydrate and the Sodium carbonate decahydrate at least in the mixture of anhydrous sodium carbonate and water mixing gained.
4. the method for the preparation of powdery sodium percarbonate according to claim 1 is characterized in that, is 2Na with theoretical molecular formula
2CO
33H
2O
2SPC-D be the benchmark meter, use the aqueous hydrogen peroxide solution of accurate stoichiometric quantity, add 1.49～1.52 moles aqueous hydrogen peroxide solution in every mole of yellow soda ash.
5. the method for the preparation of powdery sodium percarbonate according to claim 1 is characterized in that, the massfraction of hydrogen peroxide is 27.5%～70% in the aqueous hydrogen peroxide solution.
6. the method for the preparation of powdery sodium percarbonate according to claim 1 is characterized in that, the adding massfraction is 50%～60% 1-hydroxyl ethane-1 in the aqueous hydrogen peroxide solution, 1-Disodium alendronate solution.
7. the method for the preparation of powdery sodium percarbonate according to claim 6 is characterized in that, 1-hydroxyl ethane-1, and the quality that the 1-Disodium alendronate adds is 2%～10% of a hydrogen peroxide quality.
8. the method for the preparation of powdery sodium percarbonate according to claim 1 is characterized in that, the temperature of inlet air was selected in 110～180 ℃ when Rotatingandflashstreamingdrier was dry.
9. the method for the preparation of powdery sodium percarbonate according to claim 1 is characterized in that, Outlet Gas Temperature was controlled in 50～70 ℃ when Rotatingandflashstreamingdrier was dry.
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