CN1637128A - Process for producing detergent particle group - Google Patents
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- CN1637128A CN1637128A CN 200410102279 CN200410102279A CN1637128A CN 1637128 A CN1637128 A CN 1637128A CN 200410102279 CN200410102279 CN 200410102279 CN 200410102279 A CN200410102279 A CN 200410102279A CN 1637128 A CN1637128 A CN 1637128A
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Abstract
A method for producing the detergent particle group is provided by mixing surfactant-mixed liquid obtained by mixing at least 1 kind of anionic surfactant with molten state fatty acids (molten fatty acids), with a powdery detergent raw material containing at least 1 kind of an alkaline detergent builder. The detergent particle group obtained by the method has high volume density, capable of improving clean activity by the high concentration of surfactant component, is suitable for clothing detergent due to good solubility and free fluidity.
Description
Technical field
The present invention relates to contain the manufacture method of the detergent particle group of anion surfactant.When the tensio-active agent mixed solution that mainly contains anion surfactant mixes with powder lotion raw material, can suppress the particle alligatoring so that the manufacture method of the detergent particle group that solvability is good, free-flowing property is good of caking.
Background technology
In the manufacturing field of powder lotion, the many usually forms with the high concentration solution of anion surfactant are used, and its proterties is thick.Especially when described anion surfactant is made detergent particle as tackiness agent and powder lotion mixed raw material, cause because of its proterties, particle alligatoring even caking can occur during granulation, so that be difficult to the problem of the detergent particle that obtains granulous, have free-flowing property.
In the flat 6-506720 communique of Japanese Unexamined Patent Application Publication, disclosed the tensio-active agent mixed solution by mainly containing anion surfactant and the high-speed mixing of powder lotion raw material, keeping granulous simultaneously, make the method for free-flowing property lotion.But when carrying out mass production, the thick and heavy problem of equipment is arranged with this method, therefore still undesirable.
And in No. 3105266 patent gazette of Japan, disclosed the surfactant component that contains crystallinity and amorphism anion surfactant clean particulate manufacture method, it is at first on the basis of hybrid junctions crystallinity anionic surfactant paste and powder lotion raw material, add the amorphism anion surfactant, carry out granulation.Utilize this method to obtain, can suppress the particle alligatoring so that the particulate state lotion of caking, but because of not being in advance above-mentioned two kinds of anion surfactants to be mixed simultaneously, so, make manufacturing processed long, thus also undesirable.
Summary of the invention
Promptly, to the effect that of the present invention, at least a kind of anion surfactant mixed with the lipid acid that is the state of dissolving (dissolving lipid acid) and the tensio-active agent mixed solution, with the manufacture method of the powder lotion raw material blended detergent particle group that contains a kind of basic lotion synergistic agent (builder) at least.
When the present invention relates to mainly to contain the tensio-active agent mixed solution of anion surfactant and powder lotion raw material and mixing, need not special mechanical force and multiple working procedure, can suppress particle alligatoring and caking, make the method for the good detergent particle group of solvability and free-flowing property.
Illustrated above-mentioned and other advantage of the present invention by following explanation.
The inventor etc. are after further investigation, found that, to mainly be the heavy-gravity anion surfactant and dissolve lipid acid and mix and reach low viscous tensio-active agent mixed solution and mix with the powder lotion raw material that contains the basic lotion synergistic agent, with lipid acid neutralization wherein, can suppress the particle alligatoring significantly so that lump, thereby finish the present invention.
The manufacture method of the detergent particle group of the application of the invention can reach and need not special mechanical force, also need not multiple working procedure, can suppress the particle alligatoring so that caking, makes the effect of the lotion of the good high bulk density of solvability and free-flowing property efficiently.
Embodiment
Below, describe the present invention in detail.
The lotion raw material that the present invention is used
In the present invention, the lotion raw material uses at least a kind of anion surfactant to mix with the lipid acid that is the state of dissolving (dissolving lipid acid) and tensio-active agent mixed solution that gets and the powder lotion raw material that contains a kind of basic lotion synergistic agent at least.In the present invention, the tensio-active agent mixed solution is meant the low-viscosity (mobile) liquid shape lotion raw mix that contains above-mentioned anion surfactant and dissolve lipid acid, is made of the aftermentioned raw material.And be distributed in the powder lotion raw material when mixing for being easy to, the viscosity of this tensio-active agent mixed solution is preferably 50～15000mPas, more preferably 50～10000mPas.The measuring method of this viscosity can be enumerated the method for measuring this tensio-active agent mixed solution under the temperature when remaining on modulation with Brookfield viscometer.For measuring above-mentioned range of viscosities, can select rotor and revolution as one sees fit, be measured value to measure the reading of beginning after 1 minute.
Anion surfactant
At least contain a kind of anion surfactant in the tensio-active agent mixed solution.Anion surfactant can adopt a kind in following separately or be used in combination.Its kind can be enumerated the soap (soap) of carbonatoms 10～18, the linear alkylbenzene sulfonate (LAS) of carbonatoms 10～18, the alkyl-sulphate (AS) of carbonatoms 10～18, the alkyl alkoxy sulfate (AES) of carbonatoms 10～18 etc.Wherein, consider cleaning capacity, be preferably the LAS of carbonatoms 10～18, more preferably the LAS of carbonatoms 12.
Above-mentioned anion surfactant can be obtained by the acid precursor of this anion surfactant and the neutralization reaction of alkaline reagents (aqueous sodium hydroxide solution, potassium hydroxide aqueous solution etc.), and also can be moisture.When anion surfactant is moisture, can before neutralization reaction, adds water and/or after neutralization, add water.For the surfactant component that makes detergent particle group has high density, the water content of above-mentioned anion surfactant is preferably smaller or equal to 50 weight %, more preferably smaller or equal to 40 weight %, is preferably especially smaller or equal to 30 weight %.
Dissolve the lipid acid of state
In the present invention, the lipid acid (also be called down dissolve lipid acid) that dissolves state is meant the lipid acid that is the state of dissolving when this anion surfactant mixes, and comprises being the fused state after being in a liquid state and heating up under the normal temperature.Be used for the kind that dissolves lipid acid of the present invention and can enumerate saturated fatty acid and unsaturated fatty acids, and consider and the solidified nature of basic lotion synergistic agent, be preferably saturated fatty acid by the soap of neutralization reaction generation.The control effect of the toughness of the anion surfactant for can reach the mixing of good and powder lotion raw material the time, the average carbon atom number of saturated fatty acid is preferably more than and equals 12, and considers the reactivity worth of lipid acid, is preferably less than equaling 18.And when this lipid acid was the mixture of the different lipid acid of carbonatoms (round values), average carbon atom number was meant the weighted mean of part by weight of the lipid acid of variant carbonatoms.According to above-mentioned 2 points, the saturated fatty acid of average carbon atom number 12～18 more preferably, more preferably average carbon atom number 14 and 16 saturated fatty acid.The content that dissolves lipid acid contains the viscosity of the tensio-active agent mixed solution of anion surfactant for reduction, and the particle alligatoring and the caking that suppress detergent particle group in the aftermentioned granulation are very important.For making the gained detergent particle group have good solubility, with anion surfactant is 100 weight parts, then this content is elected as again smaller or equal to 70 weight parts, more preferably smaller or equal to 60 weight parts, more preferably smaller or equal to 40 weight parts, and be particle alligatoring and the caking that suppresses in the granulation, be preferably more than and equal 5 weight parts, more preferably more than or equal to 10 weight parts.That is, according to above-mentioned two aspects, be 100 weight parts with anion surfactant, the content that dissolves lipid acid is preferably 5～70 weight parts.Anion surfactant amount among the present invention is meant effective constituent (significant quantity).
Other lotion liquid starting material
The tensio-active agent mixed solution also can contain the surfactant component outside the anion surfactants such as nonionogenic tenside.The kind of nonionogenic tenside can be enumerated Voranol EP 2001, polyoxyethylene alkyl phenyl ether etc.Preferred use carbonatoms 10～20, more preferably carbonatoms 10～15, more preferably the average addition mole number of ethylene oxide of the primary alconol of the straight or branched of carbonatoms 12～14 or secondary alcohol is 5～15, is preferably 6～12, more preferably 6～10 Voranol EP 2001.And this Voranol EP 2001 contains the alkyl oxide of more low oxidation ethylene addition mole number usually, 0～3 mole of preferred addition amount smaller or equal to 35 weight %, more preferably smaller or equal to 25 weight %.
In addition, the tensio-active agent mixed solution also can contain the water-soluble polymers with mud dispersiveness and anti-recontaminate.It is nonionic organic compound and polyoxyethylene-type nonionic organic compound that first kind water-soluble polymers can be enumerated polyethers.Specifically can enumerate polyoxyethylene glycol (PEG), polypropylene glycol etc.And consider the rerum natura of gained detergent particle group, PEG more preferably.Consider solvability, the molecular-weight average of PEG is preferably smaller or equal to 30000, more preferably smaller or equal to 15000.And consider solidified nature, be preferably more than equal 200, more preferably more than or equal to 600.
Another kind of water-soluble polymers is the organic synergistic agent.Specifically can enumerate salt, polyvinyl alcohol, carboxymethyl cellulose of polyacrylate, vinylformic acid-maleic acid etc.Wherein, according to the cleaning capacity of gained detergent particle, be preferably the salt of polyacrylate, vinylformic acid-maleic acid.And this class salt can be enumerated OLIGOMER DI-2 (trade(brand)name, Japanese Peroxide K.K. system), AQUALIC TL-500 (trade(brand)name, Japanese catalyst (strain) system) etc.
When above-mentioned water-soluble polymers was used as the lotion raw material, many usually the interpolation with powder morphology used.This be because, even the workable aqueous solution, also can because of its toughness in aforesaid granulation, bring out the particle coarse so that the caking problem.But in the present invention, above-mentioned water-soluble polymers owing to dissolve lipid acid the action effect of above-mentioned anion surfactant also is applicable to the water-soluble polymers aqueous solution, so can be made into the tensio-active agent mixed solution under the aqueous solution of drying not, secondary processing such as make powder.And the moisture ratio of the water-soluble polymers aqueous solution is preferably 30～80 weight %, more preferably 40～60 weight %.
Cooperate each material quantity with following ratio, form the tensio-active agent mixed solution, just can make and make suitable tensio-active agent mixed solution.In the tensio-active agent mixed solution, anion surfactant and the total content that dissolves lipid acid are 5～90 weight %, are preferably 15～80 weight %, more preferably 25～65 weight %; The content of nonionic surfactant is 0～85 weight %, is preferably 5～65 weight %, more preferably 15～50 weight %; The total content of water-soluble polymers is 0～40 weight %, is preferably 1～30 weight %, 3～25 weight % more preferably, and moisture is 2～40 weight %, is preferably 5～30 weight %, more preferably 10～25 weight %.
The modulation of tensio-active agent mixed solution
The blending means that is used to modulate the above-mentioned raw materials of above-mentioned tensio-active agent mixed solution can adopt known method commonly used, especially according to following interpolation order with the following apparatus modulation, can obtain required tensio-active agent mixed solution.
At first, for suppressing the formation of gelation thing, the interpolation order is preferred through the following stage.
(1) when the tensio-active agent mixed solution contains the arbitrary combination of nonionogenic tenside, first kind water-soluble polymers, other moisture, with the stage of these raw material premixs.
(2) as required, interpolation, mixed anion tensio-active agent in the mixed solution of (1), maybe with in the acid precursor of this anion surfactant and the time, be the neutralization reaction in the mixed solution of realizing (1), the stage of in the mixed solution of (1), add, mixing alkaline reagentss such as this acid precursor and aqueous sodium hydroxide solution.
(3) in the mixed solution of (2) that sufficient mixing and/or neutralization reaction are finished, add, mix the stage that dissolves lipid acid.
When (4) the tensio-active agent mixed solution contains the second class water-soluble polymers, the stage of in the mixed solution of (3), add, mixing this water-soluble polymers.
And be detained, when being stored in the groove, preferably above-mentioned (2) mixed solution the when stage finishes be stored in the storage tank at above-mentioned tensio-active agent mixed solution, soon with before powder lotion raw material mixes carrying out the stage that (3) reach (4).And finishing of (2) stage neutralization reaction can be passed through the pH value and/or the acid number of the mixed solution in this stage of mensuration and confirm.When the pH value be 10～13 and/or acid number be-3.5～-during 0.5mgKOH/g, neutralization reaction is finished.
In addition, mixing machine preferably uses the matching piece of the warm water sleeve pipe etc. that has stirring rake and be used for attemperation.And when needing neutralization as this acid precursor of above-mentioned anion surfactant, preferably equipment has and is used to the external circulating system carrying the pump of liquid and be used to remove the heat exchanger of neutralization heat on above-mentioned mixing machine.And when continuing this acid precursor of neutralization, the said external recycle system preferably has silent oscillation or driving agitator.
And the mixture temperature scope in the modulation process of above-mentioned tensio-active agent mixed solution preferably sets in maximum value～+ 15 of the softening temperature of the fusing point of above-mentioned use raw material and/or anion surfactant (corrective) ℃, more preferably is set in the scope of maximum value～+ 10 ℃ of softening temperature of the fusing point of above-mentioned use raw material and/or anion surfactant (corrective).
Because the present invention is preferably and need not specially to heat, so particularly, the temperature of said mixture is preferably 60～90 ℃, more preferably 65～85 ℃.
Secondly, in the present invention, the powder lotion raw material and the above-mentioned tensio-active agent mixed solution that also will contain at least a kind basic lotion synergistic agent use simultaneously.
The basic lotion synergistic agent
The basic lotion synergistic agent except that playing the effect of cleaning base, also plays the contained effect that dissolves the neutralizing agent of lipid acid in the tensio-active agent mixed solution in the present invention.The basic lotion synergistic agent can use a kind of in the following substances separately, or is used in combination.Its kind can be enumerated carbonate, supercarbonate, silicate etc.Specifically can enumerate yellow soda ash, salt of wormwood, sodium bicarbonate, water glass etc.Wherein, yellow soda ash is further divided into dense ash and light ash (light ash), considers and dissolve the response capacity of lipid acid, preferably uses light ash.
Carry the powder surface of holding the tensio-active agent mixed solution long-pending and inhibition particle alligatoring and caking for increasing, the particle diameter of the mixture of this class basic lotion synergistic agent is preferably 5～300 μ m, more preferably 5～200 μ m.
Because the contained lipid acid that dissolves during the addition of basic lotion synergistic agent need be enough to and in the tensio-active agent mixed solution, so be preferably 15 times of dissolving the lipid acid neutralization equivalent and more than, more preferably 20 times and more than, be preferably especially 25 times and more than, and be because of water and fixed situation take place when suppressing the preservation of gained detergent particle group, be preferably 80 times of dissolving the lipid acid neutralization equivalent and below, more preferably 70 times and below.During the neutralization equivalent that dissolves lipid acid among the present invention is meant and 1 mole of mole number that dissolves the required basic lotion synergistic agent of lipid acid.
Other powder lotion raw material
The present invention also can use other powder lotion raw material except that above-mentioned basic lotion synergistic agent.This class powder lotion raw material can be enumerated inorganic synergistic agent, extender, cleaning additive, whitening agent etc.Inorganic synergistic agent can be enumerated sulphite, tri-polyphosphate, other phosphoric acid salt, crystalline aluminosilicate, amorphous aluminosilicate etc.Specifically can enumerate S-WAT, tripoly phosphate sodium STPP, zeolite etc.And the kind of extender, cleaning additive and whitening agent can be enumerated enzyme and fluorescence dyes such as saltcake, proteolytic enzyme, cellulase respectively.
The used powder lotion raw material of the present invention can form above-mentioned basic lotion synergistic agent and other powder lotion raw material hybrid modulation by common method.
The manufacture method of detergent particle group
The manufacture method of detergent particle group of the present invention has above-mentioned tensio-active agent mixed solution and powder lotion raw material stirring blended operation.In the present invention,, can show and need not special mechanical force and multiple working procedure, just can suppress particle alligatoring and caking, efficiently make the effect of the good high volume density lotion of solvability and free-flowing property by making detergent particle group with this method.
Wherein, for solving the excessive agglutinative problem of the caused obstruction powder of toughness lotion raw material dispersion/powder lotion raw material of anion surfactant of the reason that also is particle alligatoring and caking simultaneously, preferably when tensio-active agent mixed solution and the mixing of powder lotion raw material, implement simultaneously and dissolve the neutralization of lipid acid and the granulation of detergent particle group.
In the present invention, the blending means of above-mentioned tensio-active agent mixed solution and powder lotion raw material can adopt known method commonly used, mixes according to the following mixing machine that uses in order especially, just can obtain required detergent particle group.
At first, be preferably the order in following stage of process.
(5) at least a kind of basic lotion synergistic agent and powder lotion raw material are in addition dropped into mixing machine, with the stage of powder lotion raw material premix.
(6) under mixing, interpolation contains the tensio-active agent mixed solution that dissolves lipid acid in the powder lotion raw material of (5), granulation when neutralization dissolves lipid acid, the stage of improving volume density.
(7) by in the mixture of (6), adding, mixing new powder lotion raw material, be covered, improve the stage of the free-flowing property of detergent particle group on the mixture surface of (6).
In the present invention, because above-mentioned reason can suppress particle alligatoring and caking in (6), and by transferring to suitable temperature condition, mixing condition, just can make more suitably detergent particle group.Therefore, the used mixing machine of the present invention preferably uses the cold warm water telescopic mixing machine that has stirring rake and can adjust temperature.Manufacture also is not limited to any in batch-type, the continous way, and various suitable mixing machine forms can be enumerated following several.
When mixing with batch-type, preferably following (a) and equipment (b).
(a) be that stir shaft is arranged in the tempering tank, the stirrer that stirring rake carries out powder mixes is housed on the axle.Henschel stirrer (Mitsui three pond chemical industry machines (strain) system) for example; homogenizer (dark river industry (strain) system); vertical granulator ((strain) Powrex system) etc.; be preferably especially in horizontal tempering tank; in cylinder center stir shaft is arranged; the stirrer that stirring rake carries out powder mixes is housed, L dige stirrer (Matuzaka skill grind (strain) system) for example, Plough Share stirrer (Pacific Ocean machine worker (strain) system) on the axle.
(b) carry out the blended stirrer by the rotation that in fixed semi-cylindrical shaped container, forms the banded oar of spiral, for example ribbon blender (only powder (strain) system).
When stirring, be preferably the equipment of following (c)～(e) with continous way.
(c) comprise vertical cylinder with powder dog-house and the main shaft with mixing blade, main shaft is supported by upper bearing, discharges the continuous mixers that side is the free state structure, for example FlexoMix type (strain) Powrex system).
(d) drop into raw material on top, make this plectane high speed rotating, utilize shearing action to carry out the blended stirrer, Flow Jet stirrer ((strain) skill is ground the Powtechs system) for example, screw pin stirrer (Pacific Ocean machine worker (strain) system) with the plectane that stirs bolt.
(e) have stir shaft in the tempering tank, the continuous mixers that stirring rake carries out powder mixes is housed on the axle.For example continuous Henschel stirrer (Mitsui three pond chemical industry machines (strain) system).Homogenizer (dark river industry (strain) system), vertical granulator devices such as ((strain) Powrex systems) also can be used as continuous apparatus.Be preferably especially in horizontal tempering tank, stir shaft arranged, the continuous mixer that stirring rake carries out powder mixes is housed on the axle, L dige stirrer (Matuzaka skill grind (strain) system) for example, Plough Share stirrer (Pacific Ocean machine worker (strain) system) in cylinder center
Said apparatus also can be provided with to have more than 1 and be used to pulverize the pulverizer of aggegation at the pulverizing oar of the detergent particle of tempering tank inside.Also can be provided for making the air-supply arrangement and the gas barrier of cold wind circulation in the tempering tank.
And, add, so preferably be provided with the pipeline of band micronize nozzle in the tempering tank owing to the tensio-active agent mixed solution is preferably with atomize in the stage of above-mentioned (6).
And when carrying out, availablely carry out each stages of above-mentioned (5)～(7) successively with a kind of mixing machine with batch-type, after the also available stage of carrying out (5) and (6) with a kind of mixing machine successively, carry out the stage of (7) with other mixing machine.When carrying out with continous way, can use the stage of carrying out (5) and (6) with a kind of mixing machine simultaneously, carry out the stage of (7) again with other mixing machine.
Mixing condition when carrying out each stages of above-mentioned (5)～(7) can be shown with the defined Froude numerical table of following formula.
Fr＝V
2/(R×g)
Fr represents that Froude number, V represent that circumferential speed (m/s), the R of stirring rake or pulverizing blade tip end represent the rotation radius (m) of stirring rake or pulverizing oar, and g represents universal gravity constant (m/s
2).
For making powder lotion raw material form the uniform state of appropriateness, the mixing condition in (5) stage is preferably, and the Froude number of main stirring rake is 0.5～5, is preferably 0.8～3; During for pulverizer, the Froude number of pulverizing oar is 500～2000, is preferably 800～1500.And mixing time is preferably 0.5～4 fen, more preferably 1～3 minute.
Excessive for preventing because of the shearing granulation, the Froude number that the mixing condition when carrying out the stage of (6) or carrying out (5) and (6) simultaneously is preferably main stirring rake is 0.3～4, is preferably 0.5～3; During for pulverizer, the Froude number of pulverizing oar is 0～1500, is preferably 0～500.
When carrying out with batch-type, the interpolation time of tensio-active agent mixed solution is 1～15 minute, is preferably 2～10 fens, comprises that the mixing time of the interpolation time of tensio-active agent mixed solution is 5～20 minutes, is preferably 8～15 fens.And when carrying out with continous way, its residence time is 5～20 minutes, is preferably 8～15 fens.
In addition, temperature condition in these stages is very important to the toughness that suppresses anion surfactant, and the temperature of the tensio-active agent mixed solution during interpolation, mixing machine telescopic water temperature, the temperature etc. of wind pushing air is preferably as described below when having air-supply arrangement.
Tensio-active agent mixeding liquid temperature during interpolation is preferably in above-mentioned modulation process temperature range.
Mixing machine telescopic water temperature is preferably 15～50 ℃, is preferably 20～40 ℃.When mixing machine connected air-supply arrangement, the wind pushing air temperature was 10～30 ℃, is preferably 15～25 ℃, and wind pushing air humidity is 30～90RH%, is preferably 40～80RH%, and the wind pushing air flow is that mixing machine per unit volume is 50～550Nm
3/ hr is preferably 100～500Nm
3/ hr.
In the stage of (6), the sleeve pipe water temperature of mixing machine is located at below the used fusing point that dissolves lipid acid sometimes.Even this moment, the used tensio-active agent mixed solution of the present invention is also aqueous because of not solidifying, being, and has the advantage that can carry out neutralization reaction with good operability.
In addition, in the stage of (6), dissolve lipid acid neutralization and finish the moment that a little no longer produces neutralization heat, this can be by measuring the powder layer temperature in the mixing machine in time, the moment affirmation of no longer rising with temperature.
Newly add powder lotion raw material and overlay on the mixture of (6) for making, (7) mixing condition in stage is preferably, and the Froude number of main stirring rake is 0.3～4, is preferably 0.5～3, the Froude number of the pulverizing oar when having pulverizer is 500～2000, is preferably 800～1500.And mixing time is preferably 0.5～4 fen, more preferably 1～3 minute.In addition, so long as those skilled in the art, just know that this stage usedly newly adds powder lotion raw material what this uses, be preferably micro mist, preferably adopt the particle of primary particle diameter smaller or equal to 10 μ m.For example, the powder lotion raw material outside the above-mentioned basic lotion synergistic agent can be enumerated crystalline aluminosilicate, amorphous aluminosilicate etc.Specifically be preferably zeolite.
For making suitable detergent particle group, in the manufacture method of detergent particle group of the present invention, when regulating each lotion material quantity, the use level of tensio-active agent mixed solution is selected 15～45 weight parts for use, is preferably 20～40 weight parts, more preferably 25～35 weight parts; The use level of basic lotion synergistic agent is selected 10～45 weight parts for use, be preferably 15～40 weight parts, 20～35 weight parts more preferably, the powder lotion raw material use level outside the basic lotion synergistic agent is selected 10～75 weight parts for use, be preferably 20～65 weight parts, more preferably 30～55 weight parts.
The detergent particle group that obtains as stated above preferably satisfies the particle swarm of following rerum natura.
(i) volume density: consider the solvability of gained detergent particle group, preferably smaller or equal to 1200g/L, more preferably 600～1200g/L, more preferably 700～1000g/L.
(ii) median size: be preferably 250～800 μ m, more preferably 300～600 μ m.Consider the solvability of gained detergent particle group, be preferably, equal 250 μ m for suppressing that dust takes place, being preferably more than smaller or equal to 800 μ m.Median size is used JIS Z 8801 standard sieves, after vibration 5 minutes, according to number particle diameter in the weight fraction mensuration of different mesh sizes.
(iii) mobile: consider the operability of gained detergent particle group, flowing time is preferably smaller or equal to 10 seconds, more preferably smaller or equal to 8 seconds.Flowing time is to measure the required time of powder of flowing out 100mL with hopper from the volume density of JIS K 3362 defineds.
(iv) solvability:, be more preferably less than and equal 0.5% preferably smaller or equal to 1.0%.The 0.83g that materialses adds in 10 ℃, 1 liter the pipeline water, stir 10 minutes with the magnetic stirrer after, with 200 purpose metal mesh filters, represent solvability with the surplus ratio (%) of dry after-filtration.
And that the production performance index is preferably is as follows.
(v) yield: with the gained detergent particle group is 100 weight %, and the ratio by 1180 μ m sieve is more than the 60 weight %, is preferably more than the 70 weight %.
According to the detergent particle group that the inventive method obtains, the volume density height can effectively improve cleaning action by the high densityization of surfactant component, and because mobile, solvability is good, is applicable to laundry detergent.
Embodiment
Specifically describe, disclose embodiments of the present invention below by embodiment.But these embodiment only are of the present invention illustrating, and do not constitute the qualification to invention.
In addition, in the following embodiments, the acid precursor of the alkyl benzene sulphonate (ABS) sodium salt of anion surfactant uses Witco 1298 Soft Acid, and the acid precursor of fatty acid sodium salt uses the mixture of the saturated fatty acid of average carbon atom number 14～18.
And nonionogenic tenside uses polyoxyethylene lauryl ether, and the average addition mole number of use ethylene oxide is 6 material.
And using the material of 100 weight % of the aqueous solution of 60 weight % of molecular-weight average 13000 and molecular-weight average 200 as the polyoxyethylene glycol of water-soluble polymers, acrylic-maleic copolymer salt uses the 40 weight % aqueous solution of Japanese catalyst (strain) system.
And the lipid acid that dissolves that is mixed in the tensio-active agent mixed solution uses tetradecanoic acid (LUNACMY-98), flower king (strain) system) or palmitinic acid (LUNAC P-95, flower king (strain) system).
And the lotion synergistic agent of alkalescence---light ash and sodium bicarbonate adopt the product of Japanese eastern Cao (strain) system.Light ash (median size 10 μ m) is that the raw material body (median size 100 μ m) of light ash is pulverized and got with Japanese only powder system spraying gun.
In addition, be other powder lotion raw material with PQ CHEMICALS system 4A type zeolite.
In addition, the fusing point of used lipid acid etc. among the following embodiment, polyoxyethylene glycol (PEG13000) is 55 ℃, is in a liquid state under the PEG200 normal temperature, and tetradecanoic acid is 55 ℃, and palmitinic acid is 63 ℃.
Embodiment 1
Described 9.7 weight part polyoxyethylene glycol (PEG200) of table 1 and 1 weight part PEG13000 (moisture 1.7 weight parts) are heated mixing down at 60 ℃, add the aqueous sodium hydroxide solution of 48 weight %, with alkyl benzene sulphonate (ABS) neutralization, the mixed solution of furnishing sodium alkyl benzene sulfonate growing amount 13.4 weight parts.The abundant acid precursor (alkyl benzene sulphonate (ABS)) of the above-mentioned anion surfactant of pre-neutralization so that the lipid acid that dissolves that add the back is not neutralized, and adjusted and is respectively become component, makes sodium hydroxide unlikely residual excessive.This mixed solution is remained under 75 ℃, add mixed palmitinic acid 2.4 weight parts that dissolve, obtain containing the tensio-active agent mixed solution that dissolves lipid acid.
In addition, in L dige stirrer (the Matuzaka skill is ground (strain) system, 130 liters of capacity, band sleeve pipe), drop into and pulverize light ash 33 weight parts, sodium bicarbonate 7.9 weight parts, 4A type zeolite 28.7 weight parts begin to stir.Stir with main shaft (55r/min, Fr=0.85) and knife mill (chopper, 3600r/min, Fr=1088) carry out, to the water of 20 ℃ of sleeve pipe feedings, mixed powder lotion raw material is after 1 minute, in 6 minutes, add above-mentioned tensio-active agent mixed solution, stop to stir and discharging.The evaluation result of the detergent particle group that obtains thus is shown in table 1.
Embodiment 2
Described 10.2 weight part nonionogenic tensides of table 1 and 1 weight part polyoxyethylene glycol (moisture 1.7 weight parts) are heated mixing down at 60 ℃, add the aqueous sodium hydroxide solution of 48 weight %, with alkyl benzene sulphonate (ABS) neutralization, the mixed solution of furnishing sodium alkyl benzene sulfonate growing amount 12.1 weight parts.Heat down in 80 ℃ again and mix above-mentioned mixed solution, add the aqueous sodium hydroxide solution of 48 weight %,, generate the fatty acid sodium salt (soap) of 2 weight parts with the lipid acid neutralization.The abundant acid precursor of the above-mentioned anion surfactant of pre-neutralization (alkyl benzene sulphonate (ABS), average carbon atom number 14～18 saturated fatty acid) so that the lipid acid that dissolves that add the back is not neutralized, and adjusted and is respectively become component, makes sodium hydroxide unlikely residual excessive.This mixed solution is remained under 75 ℃, add mixed palmitinic acid 1 weight part that dissolves, obtain containing the tensio-active agent mixed solution that dissolves lipid acid.
In addition, in L dige stirrer (the Matuzaka skill is ground (strain) system, 130 liters of capacity, band sleeve pipe), drop into and pulverize light ash 27.4 weight parts, sodium bicarbonate 6.1 weight parts, 4A type zeolite 24.4 weight parts begin to stir.Stir and carry out, feed 20 ℃ water to sleeve pipe with main shaft (55r/min) and knife mill (3600r/min).Mixed powder lotion raw material added above-mentioned tensio-active agent mixed solution after 1 minute in 10.5 minutes, continue then to stir 1 minute.Then in 0.5 minute, add vinylformic acid-maleic acid 1.5 weight parts (moisture 3.8 weight parts), continue afterwards to stir 1.5 minutes.Add 4A type zeolite 8.1 weight parts again, stir after 1 minute and discharge as surface-coated dose.The evaluation result of the detergent particle group that obtains thus is shown in table 1.
Embodiment 3
Described 9.5 weight part nonionogenic tensides of table 1 and 0.5 weight part polyoxyethylene glycol (moisture 0.8 weight part) are heated mixing down at 60 ℃, add the aqueous sodium hydroxide solution of 48 weight %, in and alkyl benzene sulphonate (ABS), the mixed solution of furnishing sodium alkyl benzene sulfonate growing amount 12.6 weight parts.The abundant acid precursor (alkyl benzene sulphonate (ABS)) of the above-mentioned anion surfactant of pre-neutralization so that the lipid acid that dissolves that add the back is not neutralized, and adjusted and is respectively become component, makes sodium hydroxide unlikely residual excessive.This mixed solution is remained under 65 ℃, add mixed tetradecanoic acid 3.2 weight parts that dissolve, obtain containing the tensio-active agent mixed solution that dissolves lipid acid.
In addition, in L dige stirrer (the Matuzaka skill is ground (strain) system, 130 liters of capacity, band sleeve pipe), drop into and pulverize light ash 28.4 weight parts, sodium bicarbonate 6.3 weight parts, 4A type zeolite 23.8 weight parts begin to stir.Stir and carry out, feed 20 ℃ water to sleeve pipe with main shaft (55r/min) and knife mill (3600r/min).Mixed powder lotion raw material added above-mentioned tensio-active agent mixed solution after 1 minute in 4.5 minutes, stir after 2 minutes, then added vinylformic acid-maleic acid 1.6 weight parts (moisture 4 weight parts) in 0.5 minute, continued afterwards to stir 1.5 minutes.Add 4A type zeolite 8.4 weight parts again, stir after 1 minute and discharge as surface-coated dose.The evaluation result of the detergent particle group that obtains thus is shown in table 1.
Embodiment 4
Remove and use the lipid acid that dissolves among the embodiment 3 instead tetradecanoic acid by palmitinic acid, the temperature condition that dissolves lipid acid that adds when mixing in the tensio-active agent mixed solution changes into outside 75 ℃ by 65 ℃, carries out operation similarly to Example 3.The evaluation result of the detergent particle group that obtains thus is shown in table 1.
Embodiment 5
Described 9.5 weight part nonionogenic tensides of table 1 and 0.5 weight part polyoxyethylene glycol (moisture 0.8 weight part) are heated mixing down at 60 ℃, add the aqueous sodium hydroxide solution of 48 weight %, in and alkyl benzene sulphonate (ABS), the mixed solution of furnishing sodium alkyl benzene sulfonate growing amount 12.6 weight parts.The abundant acid precursor (alkyl benzene sulphonate (ABS)) of the above-mentioned anion surfactant of pre-neutralization so that the lipid acid that dissolves that add the back is not neutralized, and adjusted and is respectively become component, makes sodium hydroxide unlikely residual excessive.This mixed solution is remained under 75 ℃, add mixed palmitinic acid 3.2 weight parts that dissolve, obtain containing the tensio-active agent mixed solution that dissolves lipid acid.In this tensio-active agent mixed solution, add mixed vinylformic acid-maleic acid 1.6 weight parts (moisture 4 weight parts) again, keep 75 ℃.
In addition, in L dige stirrer (the Matuzaka skill is ground (strain) system, 130 liters of capacity, band sleeve pipe), drop into and pulverize light ash 28.4 weight parts, sodium bicarbonate 6.3 weight parts, 4A type zeolite 23.8 weight parts begin to stir.Stir and carry out, feed 20 ℃ water to sleeve pipe with main shaft (55r/min) and knife mill (3600r/min).Mixed powder lotion raw material added above-mentioned tensio-active agent mixed solution after 1 minute in 4.5 minutes, stir after 3 minutes.Then add 4A type zeolite 8.4 weight parts, stir after 1 minute and discharge as surface-coated dose.The evaluation result of the detergent particle group that obtains thus is shown in table 1.
Embodiment 6
Ratio of components and operation with same with embodiment 5 obtain containing the tensio-active agent mixed solution that dissolves lipid acid and vinylformic acid-maleic acid.
In addition, in L dige stirrer (the Matuzaka skill is ground (strain) system, 130 liters of capacity, band sleeve pipe), drop into and pulverize light ash 28.4 weight parts, sodium bicarbonate 6.3 weight parts, 4A type zeolite 23.8 weight parts begin to stir.Stir and carry out (knife mill stops), feed 30 ℃ water to sleeve pipe with main shaft (55r/min).Mixed powder lotion raw material added above-mentioned tensio-active agent mixed solution after 1 minute in 5.5 minutes, carry out 10.5 minutes stirring afterwards.Then add 4A type zeolite 8.4 weight parts, stir after 1 minute and discharge as surface-coated dose.The evaluation result of the detergent particle group that obtains thus is shown in table 1.
Comparative example 1
Described 10.4 weight part polyoxyethylene glycol (PEG200) of table 1 and 1 weight part PEG13000 (moisture 1.7 weight parts) are heated mixing down at 60 ℃, add the aqueous sodium hydroxide solution of 48 weight %, in and alkyl benzene sulphonate (ABS), the mixed solution of furnishing sodium alkyl benzene sulfonate growing amount 14.7 weight parts.The fully acid precursor (alkyl benzene sulphonate (ABS)) of the above-mentioned anion surfactant of pre-neutralization, and adjustment respectively becomes component, makes sodium hydroxide unlikely residual excessive.This mixed solution is remained under 75 ℃, do not contained the tensio-active agent mixed solution that dissolves lipid acid.
In addition, in L dige stirrer (the Matuzaka skill is ground (strain) system, 130 liters of capacity, band sleeve pipe), drop into and pulverize light ash 33.1 weight parts, sodium bicarbonate 7.9 weight parts, 4A zeolite type 28.8 weight parts begin to stir.Stir with main shaft (55r/min) and knife mill (3600r/min), to the water of 20 ℃ of sleeve pipe feedings, mixed powder lotion raw material added above-mentioned tensio-active agent mixed solution after 1 minute in 6 minutes, feed intake finish after at once in the pasty state or block, fail to obtain having the detergent particle of free-flowing property.Only this mixture solvability evaluation result is shown in table 1.
Comparative example 2
Described 10 weight part nonionogenic tensides of table 1 and 1 weight part polyoxyethylene glycol (moisture 1.7 weight parts) are heated mixing down at 60 ℃, add the aqueous sodium hydroxide solution of 48 weight %, in and alkyl benzene sulphonate (ABS), the mixed solution of furnishing sodium alkyl benzene sulfonate growing amount 11.9 weight parts.Heat down in 80 ℃ again and mix above-mentioned mixed solution, add the aqueous sodium hydroxide solution of 48 weight %,, generate the fatty acid sodium salt (soap) of 2 weight parts with the lipid acid neutralization.The fully acid precursor of the above-mentioned anion surfactant of pre-neutralization (alkyl benzene sulphonate (ABS), average carbon atom number 14～18 gets saturated fatty acid), and adjustment respectively becomes component, makes sodium hydroxide unlikely residual excessive.This mixed solution is remained under 75 ℃, obtain containing the tensio-active agent mixed solution that dissolves lipid acid.
In addition, in L dige stirrer (the Matuzaka skill is ground (strain) system, 130 liters of capacity, band sleeve pipe), drop into and pulverize light ash 26.9 weight parts, sodium bicarbonate 6 weight parts, 4A type zeolite 26.8 weight parts begin to stir.Also have, stir and carry out, feed 20 ℃ water to sleeve pipe with main shaft (55r/min) and knife mill (3600r/min).Mixed powder lotion raw material added above-mentioned tensio-active agent mixed solution after 1 minute in 12 minutes, continue then to stir 0.5 minute.Then in 0.5 minute, add vinylformic acid-maleic acid 1.5 weight parts (moisture 3.8 weight parts), continue afterwards to stir 0.5 minute.Add 4A type zeolite 7.9 weight parts again, stir after 1 minute and discharge as surface-coated dose.The evaluation result of the detergent particle group that obtains thus is shown in table 1.
Table 1
Result according to table 1, the embodiment 1～6 that use contains the tensio-active agent mixed solution that dissolves lipid acid compares with not using the comparative example 1,2 that contains the tensio-active agent mixed solution that dissolves lipid acid, mobile, solvability is better, can obtain the detergent particle group of high volume density with high yield.
The detergent particle group that uses method of the present invention to obtain has high volume density, can effectively improve cleaning action by the high densityization of surfactant component, and because of mobile, solvability is good, the applicable laundry detergent of doing.
Therefore, by described the present invention as can be known, can obtain same material by the several different methods conversion.These conversion should not be considered as exceeding purpose of the present invention and scope, and because of to those skilled in the art, this class conversion obviously all is included within the scope of the present invention.
Table 1
| Embodiment | Comparative example | ||||||||||
| 1 | 2 | 3 | 4 | 5 | 6 | 1 | 2 | ||||
| Detergent particle Group composition weight portion | Tensio-active agent | Anion surfactant | Sodium dodecylbenzene sulfonate | 13.4 | 12.1 | 12.6 | 12.6 | 12.6 | 12.6 | 14.7 | 11.9 |
| Sodium soap (soap) | - | 2.0 | - | - | - | - | - | 2.0 | |||
| Nonionogenic tenside | Polyoxyethylene lauryl ether | - | 10.2 | 9.5 | 9.5 | 9.5 | 9.5 | - | 10.0 | ||
| Water-soluble polymers | Polyoxyethylene glycol | PEG13000 | 1.0 | 1.0 | 0.5 | 0.5 | 0.5 | 0.5 | 1.0 | 1.0 | |
| PEG200 | 9.7 | - | - | - | - | - | 10.4 | - | |||
| Vinylformic acid/maleic acid | Tensio-active agent mixed solution component | - | - | - | - | 1.6 | 1.6 | - | - | ||
| Other adds component | - | 1.5 | 1.6 | 1.6 | - | - | - | 1.5 | |||
| Moisture adds up to | 3.7 | 6.2 | 5.7 | 5.7 | 5.7 | 5.7 | 4.0 | 6.0 | |||
| Lipid acid | Tetradecanoic acid (55 ℃ of fusing points) | - | - | 3.2 | - | - | - | - | - | ||
| Palmitinic acid (63 ℃ of fusing points) | 2.4 | 1.0 | - | 3.2 | 3.2 | 3.2 | - | - | |||
| The basic lotion synergistic agent | Pulverize light ash (median size 10 μ m) | 33.0 | 27.4 | 28.4 | 28.4 | 28.4 | - | 33.1 | 26.9 | ||
| Light ash (median size 100 μ m) | - | - | - | - | - | 28.4 | - | - | |||
| Sodium bicarbonate | 7.9 | 6.1 | 6.3 | 6.3 | 6.3 | 6.3 | 7.9 | 6.0 | |||
| Other powder lotion raw material | Zeolite 4A type | 28.7 | 24.4 | 23.8 | 23.8 | 23.8 | 23.8 | 28.8 | 26.8 | ||
| Surface-coated dose | Zeolite 4A type | - | 8.1 | 8.4 | 8.4 | 8.4 | 8.4 | - | 7.9 | ||
| Tensio-active agent viscosity of mixed liquid (mPas) 1) | 60 | 2780 | 82 | 110 | 538 | 506 | 72 | 4290 | |||
| Powder layer temperature (maximum value in the granulation) (℃) | 41 | 35 | 43 | 47 | 50 | 49 | 42 | 35 | |||
| Rerum natura | Yield (the following size particles ratio of 1180 μ m weight %) | 66 | 87 | 70 | 70 | 83 | 60 | Can not granulating | 44 | ||
| Volume density (g/L) | 765 | 782 | 863 | 830 | 831 | 854 | 784 | ||||
| Mobile (sec) | 8.2 | 8.5 | 6.8 | 7.6 | 8.0 | 7.3 | 6.8 | ||||
| Median size (μ m) | 777 | 331 | 560 | 607 | 376 | 688 | 1126 | ||||
| Solvability (%) | 0.3 | 0.0 | 0.0 | 0.3 | 0.1 | 0.5 | 9.4 | 0.0 | |||
1) mixture viscosity when fatty acids or water-soluble polymers
Claims (5)
1. the manufacture method of detergent particle group is characterized in that, has
At least a kind of anion surfactant mixed with the lipid acid that is the state of dissolving (molten fat acid) and the tensio-active agent mixed solution, with the powder lotion raw material blended operation that contains a kind of basic lotion synergistic agent at least.
2. the manufacture method of detergent particle group as claimed in claim 1 is characterized in that, is 100 weight parts with anion surfactant, and the use level of described molten fat acid is 50～70 weight parts.
3. the manufacture method of detergent particle group as claimed in claim 1 is characterized in that, the use level of described basic lotion synergistic agent is more than described 15 times of dissolving the lipid acid neutralization equivalent reach.
4. the manufacture method of detergent particle group as claimed in claim 1 is characterized in that, describedly dissolves the saturated fatty acid that lipid acid is average carbon atom number 12～18.
5. manufacture method as claimed in claim 1 is characterized in that, the tensio-active agent mixed solution contains at least a kind that is selected from nonionogenic tenside, water-soluble polymers and composition thereof.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2003417112A JP4358613B2 (en) | 2003-12-15 | 2003-12-15 | Method for producing detergent particles |
| JP2003417112 | 2003-12-15 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1637128A true CN1637128A (en) | 2005-07-13 |
| CN100494332C CN100494332C (en) | 2009-06-03 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2004101022790A Expired - Fee Related CN100494332C (en) | 2003-12-15 | 2004-12-15 | Process for producing detergent particle group |
Country Status (2)
| Country | Link |
|---|---|
| JP (1) | JP4358613B2 (en) |
| CN (1) | CN100494332C (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103003404A (en) * | 2010-07-27 | 2013-03-27 | 荷兰联合利华有限公司 | Detergent composition |
| CN111171967A (en) * | 2020-01-09 | 2020-05-19 | 广州市日用化学工业研究所有限公司 | Effervescent washing product with high disintegration speed and easy rinsing and preparation method thereof |
-
2003
- 2003-12-15 JP JP2003417112A patent/JP4358613B2/en not_active Expired - Fee Related
-
2004
- 2004-12-15 CN CNB2004101022790A patent/CN100494332C/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103003404A (en) * | 2010-07-27 | 2013-03-27 | 荷兰联合利华有限公司 | Detergent composition |
| CN111171967A (en) * | 2020-01-09 | 2020-05-19 | 广州市日用化学工业研究所有限公司 | Effervescent washing product with high disintegration speed and easy rinsing and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2005171203A (en) | 2005-06-30 |
| CN100494332C (en) | 2009-06-03 |
| JP4358613B2 (en) | 2009-11-04 |
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