JP3527767B2 - Method for producing high bulk density granular detergent - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION [0001] BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for adhering a detergent to a granulator.
The present invention relates to a method for producing a granular detergent having a high bulk density by preventing the occurrence of the detergent. [0002] 2. Description of the Related Art High bulk density using a granulator having a stirring shaft
Detergent is manufactured by a general granulation method,
080, JP-A-61-69897 and JP-A-61-69897.
-69898, 61-69900, etc.
It is widely known as disclosed. these
Is an effective production method for producing high bulk density granulated detergent
However, while crushing the particles,
Extensive particle size distribution of detergent particles due to granulation characteristics
The feature is that it covers the surroundings. In this granulation method,
The particle strength of the mist-dried product is strong enough not to be overcrushed during granulation
It is required to have a degree. When the particle strength is weak
On the other hand, during granulation, a large amount of fine powder is generated
Granulation does not progress, and furthermore, particles adhere to the inner wall of the granulator.
Disadvantages that hinder the rotation of the stirring shaft and cause inoperability itself
I will. [0003] The present invention has a stirring shaft.
Of the production of high bulk density granular detergents using a rotating granulator
To prevent adhesion to the inner wall of the equipment for good granulation.
The purpose is to. [0004] SUMMARY OF THE INVENTION The present inventors have found such disadvantages.
As a result of intensive research to solve
By throwing in and granulating before spray-drying detergent,
Check that adhesion to the equipment is prevented and a good granulated detergent is obtained.
The present invention has been made. That is, the high bulk density of the present invention
The method for producing a granular detergent uses a granulating device having a stirring shaft.
100 parts by weight of spray-dried washing
The weight ratio of silicon dioxide / aluminosilicate to agent particles is
Anti-adhesive agent 3 to 10 in the range of 3/100 to 3/10
It is characterized in that parts by weight are added and mixed in the apparatus in advance. [0005] DETAILED DESCRIPTION OF THE INVENTION The present invention has a stirring shaft used in the present invention.
As a granulation device, a high-speed mixer (stirring rolling mill)
Granulator) and Henschel mixer (high-speed stirring granulator)
Type stirring granulator, Ladyge mixer (Ladyge) and
Paltan Luzer (Fuji Paudal Co., Ltd.), Pagumi
A horizontal stirring granulator such as Kisa (Fuji Powder Co., Ltd.)
It can be used, preferably a rigid stirring granulator is used. Book
The invention relates to the production using spray-dried detergent particles as a raw material.
In advance, a specific proportion of zeolite fine powder and silicon dioxide
By adding the powder to the bottom of the stirring granulator, the stirring blades
Of detergent agglomerates on the gap between the machine and the inner wall and bottom of the equipment
It is a method characterized by doing. [0006] Silicate content in spray-dried detergent particles.
Is less than 10%, the particle strength is low,
The fine powder is generated by the agitation of the particles, and the particles adhere to the inner wall of the granulator.
Occurs and hinders rotation of the stirring shaft.
Low particle strength with less than 10% silicate in smooth spray-dried particles
It has a remarkable adhesion-preventing effect even when using fine particles. Book
Silicon dioxide useful as an anti-adhesion agent according to the invention can be used on the surface of particles.
The product has a very large volume and a high lubrication effect.
Widely used as an adsorbent for liquid components in powders and powders
Have been. This is added to the stirring granulator in advance and granulated.
Is effective in preventing adhesion to the granulator.
You. The zeolite fine powder has the general formula Na_TwoO ・ Al_Two
O_Three・ MSiO_Two・ NH_TwoO (m: 1.8 to 3.0, n: 1
6) crystalline aluminosilicate represented by
It is used in clothing detergents as a chelating agent for trapping.
The primary particle size is mainly from 0.5 to 10 μm.
Also known as a modifier to improve the flowability of detergent particles
ing. When this is added to the device in advance and granulated,
Equipment adhesion is reduced. The anti-adhesion agent used in the present invention is
The ratio of silicon oxide to zeolite fine powder is 3/100 by weight.
３3/10. Silicon dioxide
When the ratio is higher than 3/10, the detergent fabric is crushed.
Poor granulation, on the other hand, Zeola than 3/100
The higher the fine powder ratio, the lower the device adhesion
However, a large amount of compounding is required to completely prevent adhesion.
I do. Because zeolite is insoluble in water,
When used for laundry, it adheres to the item to be washed,
The feeling of use is significantly impaired, which is not preferable. In the present invention,
More preferably, the component ratio of the antiadhesive is silicon dioxide / ze.
Olite = 1/10 to 2/10. Using this anti-adhesion agent, the following method is used.
When granulated, a good granulated product is obtained. First, silicon dioxide
Element and zeolite fine powder are added to a granulator in advance. This
At the time of carbonate, sulfate, silicate, or polycarboxylic acid
Continue adding inorganic powder such as salt or organic powder.
You may. At this time, stirring may be performed if necessary.
After that, spray-drying detergent is charged and binder is stirred while stirring.
And granulation is carried out to obtain a good granulated product. this
As a result, it becomes a problem when the anti-adhesion agent is not added.
No longer adheres to the device. Spray-dried detergent particles
At least one surfactant and at least one surfactant
Those containing a builder are used. [0010] For the spray-dried detergent particles in the present invention
The following are examples of surfactants that can be used. 1. Straight chain having an alkyl group having an average of 10 to 16 carbon atoms
Or branched alkyl benzene sulfonate 2. Straight chain having an alkyl group having an average of 10 to 20 carbon atoms
Or having a branched alkyl or alkenyl group,
An average of 0.5 to 8 moles of ethylene oxide per molecule
Or butylene oxide or ethylene oxide /
Propylene oxide = 0.1 / 9.9 to 9.9 / 0.9.
1 or ethylene oxide / butylene oxalate
Alkyl or alkenyl ether added by the same ratio
Sulphate 3. Alkyl group or alkene having an average of 10 to 20 carbon atoms
Alkyl or alkenyl sulfate having a nil group 4. O having an average of 10 to 20 carbon atoms in one molecule
Lefin sulfonate 5. A molecule having an average of 10 to 20 carbon atoms in one molecule.
Lucane sulfonate 6. Saturation having an average of 10 to 24 carbon atoms in one molecule
Japanese or unsaturated fatty acid salt 7. Alkyl group or alkene having an average of 10 to 20 carbon atoms
0.5 to 8 moles of ethylene in one molecule
Oxide or butylene oxide or ethylene
Oxide / propylene oxide = 0.1 / 9.9
~ 9.9 / 0.1 or ethylene oxide /
Alkyl or acetylene butylene oxide added in the same ratio
Lucenyl ether carboxylic acid 8. Α-sulfo fat represented by the following chemical formula 1
Fatty or ester salts Embedded image(Wherein Y is an alkyl group having 1 to 3 carbon atoms or a counter ion,
Z is a counter ion. R is alkyl having 10 to 20 carbon atoms
Group or alkenyl group. ) 9. The following chemical formula 2, chemical formula 3, chemical formula 4, chemical formula 5, chemical formula
Amino acid type surfactant represented by Chemical formula 6 or 7 Embedded image (Where R₁Is an alkyl group having 8 to 24 carbon atoms or alk
A kenyl group is_TwoIs hydrogen or alkyl having 1-2 carbon atoms
A group represented by R_ThreeIs an amino acid residue and X is an alkali metal or amino acid.
Shows the alkaline earth metal ions. ) [0013] Embedded image (R₁, R_TwoAnd X are as described above. n represents an integer of 1 to 5
You. ) [0014] Embedded image (R₁Is as described above. m shows the integer of 1-8. ) [0015] Embedded image (R₁, R_ThreeAnd X are as described above. R_FourIs hydrogen or carbon
Represents an alkyl or hydroxyalkyl group of Formulas 1-2
You. ) [0016] Embedded image (R₁, R_ThreeAnd X are as described above. R_FiveHas 6 to 28 carbon atoms
Β-hydroxyalkyl or β-hydroxyalkyl
Represents a nyl group. ) [0017] Embedded image (R_Three, R_FiveAnd X are as described above. ) 10. Alkyl with average carbon number of 10-20
Group or alkenyl group, from 1 to 20 moles of ethylene
Oxidized polyoxyethylene alkyl or
Is alkenyl ether 11. Having an alkyl group having an average of 6 to 12 carbon atoms,
Polyoxyethylene to which 20 mol of ethylene oxide has been added
Tylene alkyl phenyl ether 12. Alkyl group or alkyl having an average of 10 to 20 carbon atoms
1 to 20 moles of propylene oxide having a kenyl group
Polyoxypropylene alkyl or alkyl
Nyl ether 13. Alkyl group or alkyl having an average of 10 to 20 carbon atoms
Having a kenyl group, 1 to 20 moles of butylene oxide
Added polyoxybutylene alkyl or alkenyl
ether 14． Alkyl group or alkyl having an average of 10 to 20 carbon atoms
1 to 30 moles of ethylene oxa having a kenyl group in total
And propylene oxide or ethylene oxide
Nonionic Surface Activity with Addition of Butoxide and Butylene Oxide
Agents (ethylene oxide and propylene oxide or
The ratio of ethylene oxide to butylene oxide is 0.
1 / 9.9 to 9.9 / 0.1) 15. Higher fatty acids represented by the following Chemical Formula 8
Alkanolamide or alkylene oxide adduct Embedded image (Where R₁₁Is an alkyl group having 10 to 20 carbon atoms or alk
A phenyl group;₁₂Is H or CH_ThreeAnd n_ThreeIs 1
An integer between 3 and m_ThreeIs an integer of 0 to 3. ) 16. With fatty acids having an average of 10 to 20 carbon atoms
Sucrose fatty acid ester composed of sucrose 17． Fatty acids with average carbon number of 10-20 and glycerin?
Fatty acid glycerin monoester consisting of 18. An alkyl group represented by the following chemical formula 9
Minoxide Embedded image (Where R₁₃Is an alkyl group having 10 to 20 carbon atoms or alk
A phenyl group;₁₄, R₁₅Is an alkyl having 1 to 3 carbons
Is the base) 19. Chemical formula 10, chemical 11 or chemical 1 below
Betaine-type amphoteric surfactant represented by 2 Embedded image (Where R_{twenty one}Is an alkyl or alkene having 8 to 24 carbon atoms
Nil or β-hydroxyalkyl or β-hydroxy
Alkenyl group, R_{twenty two}Is an alkyl group having 1 to 4 carbon atoms, R
_{twenty three}Is alkyl or hydroxyalkyl having 1 to 6 carbon atoms
Indicates a group) [0023] Embedded image (Where R_{twenty one}And R_{twenty three}Is as described above. n_TwoIs 1-20
Represents an integer. ) [0024] Embedded image (Where R_{twenty one}And R_{twenty three}Is as described above. R_{twenty four}Has 2 to 2 carbon atoms
5 carboxyalkyl or hydroxyalkyl groups
Show. ) 20. Shown in Chemical Formula 13 or Chemical Formula 14 below
Sulfonic acid type amphoteric surfactant Embedded image (Where R₁₁Is an alkyl or alkene having 3 to 24 carbon atoms
Nyl group, R₁₂Is an alkylene group having 1 to 4 carbon atoms, R₁₃Is charcoal
An alkyl or alkenyl group having a prime number of 1 to 5 is represented by R₁₄Is charcoal
An alkylene group or oxyalkylene group having a prime number of 1 to 4
Show. ) [0026] Embedded image (Where R₁₁And R₁₄Is as described above. R₁₅, R₁₆Is carbon
Alkyl or alkenyl of the formulas 8 to 24 or 1 to 5
Group, R₁₄Is an alkylene group having 1 to 4 carbon atoms or an oxy group.
Represents a alkylene group. ) 21. Chemical formula 15, chemical 16 or chemical 1 below
Phosphate ester activator represented by 7 [Image Omitted] Alkyl (or alkenyl) acid phosphate
Steal (R is an alkyl group having 8 to 24 carbon atoms, or alkenyl
Group, n + m = 3, n = 1 to 2) [0028] Embedded image Alkyl (or alkenyl) phosphate ester
Le (R is n + m = 3, n = 1 to 3 as described above) [0029] Embedded image Alkyl (or alkenyl) phosphate ester
Le salt (R, n, and m are as described above, and M is Na, K, and Ca) 22. Shown below in Chemical Formula 18, Chemical Formula 19 or Chemical Formula 20
Cationic surfactant [0030] Embedded image (R₁, R_Two, R_Three, R_FourAt least one of which has 8 carbon atoms
~ 24 alkyl or alkenyl groups, others having 1 to 1 carbon atoms
5 represents an alkyl group. X represents a halogen. ) [0031] Embedded image (Where R₁, R_Two, R_ThreeAnd X are as described above. ) [0032] Embedded image (Where R₁, R_TwoAnd X are as described above. R_FiveIs carbon number 2
An alkylene group of 3 to 3, n_FourRepresents an integer of 1 to 20. ) The amount of the surfactant is based on the spray-dried particles.
The amount is preferably 10 to 70% by weight, more preferably
Or 25 to 50% by weight. Spray dried particles in the present invention
Inorganic builders that can be used for
There is Sodium carbonate, sesquicarbonate, sodium silicate
Alkaline salts, neutral salts such as sodium sulfate, orthophosphoric acid
Salt, pyrophosphate, tripolyphosphate, metaphosphate,
In addition to phosphates such as phytate,
Minosilicates can also be included. [0034] Embedded image x (M ′_TwoO or M "O) -Al_TwoO_Three・ Y (S
iO_Two) ・ WH_TwoO (where M ′ is an alkali metal atom, M ″
Is an alkaline earth metal atom exchangeable with calcium, x,
y and w represent the number of moles of each component, and generally, 0.7 ≦
x ≦ 1.5, 0.8 ≦ y ≦ 6, w is an arbitrary integer
You. ) Further, in the present invention, the following additives are spray-dried
Can be used for children. (1) Divalent metal ion scavenger 1. Phosphonates and their derivatives, phosphonocarboxylic
Acid salts. 2. Amino acid salts such as glutamic acid. 3. Nitrilotriacetate, ethylenediaminetetraacetate
And aminopolyacetates. 4. Polyacrylic acid, polyitaconic acid, polyfumar
Acid, polymaleic acid, maleic anhydride-acrylic acid
Polymer, dicarboxymethylcellulose, carboxyme
Non-dissociated high content such as chill cellulose and succinate
Child. 5. Polyethylene glycol, polyvinyl alcohol
, Polyvinylpyrrolidone, cold water soluble urethane poly
Non-dissociated polymers such as vinyl alcohol. 6. Diglycolic acid, oxydisuccinic acid, citric acid,
Lactic acid, tartaric acid, sucrose, lactose, raffinose, etc.
Carboxymethylated, oxalic, sulfosuccinic,
Luhuitaconic acid, malic acid, oxydisuccinic acid, gluco
Organic acid salts such as acid. (2) Anti-redeposition agent Polyethylene glycol, polyvinyl alcohol, poly
Vinylpyrrolidone, carboxymethylcellulose and the like. (3) Fluorescent whitening agent 4,4'-bis- (2-sulfostyryl) -biphenyl
Salt, 4,4'-bis- (4-chloro-3-sulfostili
B) -biphenyl salt, 2- (styrylphenyl) naphtho
Thiazole derivative, 4,4′-bis (triazole-2
-Yl) stilbene derivatives, bis (triazinylamido)
D) One or more stilbene disulfonic acid derivatives
Can be added to the composition. (4) Antioxidant Tert-butylhydroxytoluene, 4,4'-butylidene
Bis- (6-tert-butyl-3-methylphenol),
2,2′-butylidenebis- (tert-butyl-4-methyl
Phenol), monostyrenated cresol, distyrene
Cresol, monostyrenated phenol, distyrene
Phenol, 1,1′-bis-(-4-hydroxyphenyl)
Enyl) cyclohexane and the like.
Add these additives before, during, or after granulation
Can be added. (5) Inorganic salt Alkaline such as sodium carbonate, sodium sesquicarbonate and sodium silicate
Neutral salts such as sodium chloride, sodium sulfate, orthophosphate, pyrroline
Acid salt, tripolyphosphate, metaphosphate, phytate
Etc., as well as aluminosilicates. (6) Bleach Sodium percarbonate, sodium perborate, sodium sulfate peroxidation
Hydrogenated products and the like. (7) Enzyme Protease, lipase, amylase, cellulase, pea
Cutinase, maltase, saccharase and the like. (8) Anti-solidification agent Paratoluene sulfonate, xylene sulfonate, vinegar
Acid, sulfosuccinate, talc, finely divided silica,
Earth, calcium-silicate (e.g. JohnsMan
(Vill microcell etc.), magnesium oxide
etc. (9) Fragrance [0041] According to the present invention, a granulating apparatus having a stirring shaft is provided.
Effectively prevents adhesion to the stirring device during the granulation operation
And efficiently produce high bulk density detergent particles with good properties
be able to. [0042] 【Example】 ・ Spray drying A spray-dried product having the following components was obtained. Sodium linear alkyl benzene sulfonate 30 parts 1 part of sodium α-olefin sulfonate Fatty acid sodium 4 parts Nonionic surfactant 4 parts 5 parts sodium silicate Aluminosilicate 20 parts Potassium carbonate 5 parts Sodium carbonate residue 1 part of sodium polyacrylate 4 parts of water The apparent specific gravity of the obtained dried particles is 0.30 g / ml.
Was. Granulation test High-speed mixer FS-10 as a stirring granulator
(Made by Fukae Kogyo). First, install the anti-adhesion agent.
Put it in the bottom. Then, if necessary, add inorganic powder
Then, a detergent spray-dried product was added and stirred for 1 minute. this
The operating conditions at this time depend on the rotation speed of the main shaft (agitator).
420rpm, the rotation speed of the rotation shaft (chopper) on the side
It was 1900 rpm. Then, stir the binder
And granulated. It took me to put the binder
The operation was performed for 1 minute and for 7 minutes after the start of charging. Machine
Stop the machine, add the aluminosilicate powder, and 1 minute more
During operation. The input amount of spray-dried particles is 4kg,
Other powder materials and binder addition amounts are shown in Table 1 below.
Of 100%. Performed as shown in Table 1.
Examples 1 and 2 have an effective bulk specific gravity as detergent particles and
Adhesion to the inner wall did not occur and was good. [0044] [Table 1]Table 1: Raw material composition and product performance Example 1 Example 2 Comparative Example 1 Comparative Example 2 Raw material composition: wt%   Powder raw material     Silicon dioxide 0.5 0.5 0.5 0     Aluminosilicate 2.7 2.7 0 2.6     Carbonate 4.5 4.4 4.7 8.7   Spray-dried product 83.2 81.7 85.5 80.0   Binder     Aluminosilicate 1.9 2.1 2.1 2.0     Polyethylene glycol 1.3 1.4 1.1 1.0   Water 3.2 3.6 3.3 3.1 Aluminosilicate 2.7 3.6 2.8 2.6 Performance   Bulk density (g / ml) 0.70 0.75 0.61 0.65Stirrer attached No No Yes Yes

──────────────────────────────────────────────────続 き Continuation of the front page (72) Inventor Yoshikazu Fukumoto 1-3-7 Honjo, Sumida-ku, Tokyo Inside Rion Co., Ltd. (56) References JP-A-61-69898 (JP, A) JP-A Sho 61-69900 (JP, A) JP-A-4-335099 (JP, A) (58) Fields investigated (Int. Cl. ⁷ , DB name) C11D 1/00-19/00

Claims (1)

(57) [Claim 1] In the production of a detergent using a granulator having a stirring shaft, the weight ratio of silicon dioxide / aluminosilicate to 100 parts by weight of spray-dried detergent particles is used. Is 3/10
A method for producing a granular detergent having a high bulk density, characterized in that 3 to 10 parts by weight of an anti-adhesion agent in the range of 0 to 3/10 is added to an apparatus in advance and mixed.