EP0000870A1 - Procédé d'amélioration des propriétés des pâtes et poudres d'aluminosilicate de sodium - Google Patents
Procédé d'amélioration des propriétés des pâtes et poudres d'aluminosilicate de sodium Download PDFInfo
- Publication number
- EP0000870A1 EP0000870A1 EP78100496A EP78100496A EP0000870A1 EP 0000870 A1 EP0000870 A1 EP 0000870A1 EP 78100496 A EP78100496 A EP 78100496A EP 78100496 A EP78100496 A EP 78100496A EP 0000870 A1 EP0000870 A1 EP 0000870A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- dough
- aluminum silicate
- sodium
- sodium sulfate
- improving
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
- 238000000034 method Methods 0.000 title claims abstract description 8
- 239000000843 powder Substances 0.000 title claims abstract description 5
- 229910000503 Na-aluminosilicate Inorganic materials 0.000 title abstract 2
- 235000012217 sodium aluminium silicate Nutrition 0.000 title abstract 2
- 239000000429 sodium aluminium silicate Substances 0.000 title abstract 2
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 title abstract 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims abstract description 21
- 229910052938 sodium sulfate Inorganic materials 0.000 claims abstract description 21
- 235000011152 sodium sulphate Nutrition 0.000 claims abstract description 21
- 239000007787 solid Substances 0.000 claims abstract description 15
- DNEHKUCSURWDGO-UHFFFAOYSA-N aluminum sodium Chemical compound [Na].[Al] DNEHKUCSURWDGO-UHFFFAOYSA-N 0.000 claims description 17
- 239000011734 sodium Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 5
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 claims 1
- 238000001556 precipitation Methods 0.000 claims 1
- 239000007832 Na2SO4 Substances 0.000 abstract 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 abstract 1
- 229910021653 sulphate ion Inorganic materials 0.000 abstract 1
- 238000007792 addition Methods 0.000 description 13
- 239000000725 suspension Substances 0.000 description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 239000000243 solution Substances 0.000 description 6
- 238000009826 distribution Methods 0.000 description 5
- 239000003599 detergent Substances 0.000 description 4
- 238000011049 filling Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000001694 spray drying Methods 0.000 description 4
- 238000003860 storage Methods 0.000 description 4
- 230000009969 flowable effect Effects 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000002689 soil Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 229910021536 Zeolite Inorganic materials 0.000 description 2
- 239000013543 active substance Substances 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 229910052910 alkali metal silicate Inorganic materials 0.000 description 2
- 150000004645 aluminates Chemical class 0.000 description 2
- -1 aluminum silicates Chemical class 0.000 description 2
- 235000012216 bentonite Nutrition 0.000 description 2
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000011164 primary particle Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 230000000087 stabilizing effect Effects 0.000 description 2
- 239000010457 zeolite Substances 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 239000012736 aqueous medium Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 229910001388 sodium aluminate Inorganic materials 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/12—Water-insoluble compounds
- C11D3/124—Silicon containing, e.g. silica, silex, quartz or glass beads
- C11D3/1246—Silicates, e.g. diatomaceous earth
- C11D3/128—Aluminium silicates, e.g. zeolites
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
- C01B39/026—After-treatment
Definitions
- zeolite A has opened up further areas of application, such as as a builder in detergents.
- This new application places additional demands on the properties of the product.
- high whiteness e.g. Desired a small average particle diameter with a narrow grain spectrum. It is an important requirement that the product, regardless of the form in which it is present, shows the original distribution again when dispersed in water, that is to say that it has no irreversible agglomeration.
- the sodium aluminum silicate in the form of the filter dough which can be used as such in the production of detergents, has certain properties which are explained in more detail below.
- the filter dough produced in the manufacture of the sodium aluminum silicate after the mother liquor has been separated off and washed which generally contains 40-50% solids, shows a high structural viscosity in addition to other rheological anomalies. In general, this enables the dough to be pumped through without further dilution. Furthermore, due to the rheological properties mentioned, the dough can generally be stored in suitable containers and from there can be brought to flow again after the application of relatively low energy by stirring, shaking or pump suction.
- sodium sulfate not only has the advantage that it is an inexpensive component in the sodium aluminum silicate suspension is introduced, which is present in the detergent anyway, it also causes that when the dried product is dispersed in water, the sodium aluminum silicate is back in its original particle size distribution.
- Spray drying is normally used as a convenient form of further processing of the sodium aluminum silicate dough.
- spray drying has one disadvantage: the product is obtained in the form of prills.
- this inherently desirable property means that the original grain distribution in the dough does not re-establish with sufficient certainty when dispersed in water.
- the prills (30 - 80ju average diameter) often do not completely disintegrate into the original primary particles with a fineness of approx. 98 - 99% ⁇ 15 ⁇ corresponding to 95% ⁇ 10 ⁇ . This phenomenon is remedied by the addition of sodium sulfate.
- the filter dough maintained its advantageous consistency, possibly via the ge entire observation period of eight weeks. In particular, no tough, non-pumpable, non-stirrable soil body occurred. Even an addition of 1% Na 2 so 4 , based on the solid dough after the addition, already shows an effect. In practice, the addition of 2% sodium sulfate represents the lower limit. With increasing Na 2 SO 4 concentration, the effect of sodium sulfate initially increases, so that additions of 2 to 10% are expedient to improve the rheological properties. If the addition was increased by more than 10% up to 25%, based on the total solids, no rheological disadvantages were found.
- additives of more than 10%, preferably of 15-20%, based on the total solids present are required. If filter dough with N a 2 S0 4 contents of more than 10% up to approx. 25%, based on solids, is subjected to spray drying, the resulting dry products, after dispersion in water, show an extensive approximation to the original grain spectrum when determining the grain size.
- the sodium sulfate can be added at any stage in the manufacturing process of sodium aluminum silicates as long as the type of addition does not structurally change the sodium aluminum silicate itself. Furthermore, care must of course be taken that it is not removed again in a subsequent washing process. So it is e.g. It does not matter whether the sodium sulfate is already present when the sodium aluminum silicate is precipitated, i.e. whether it is added to the alkali silicate and / or the alkali aluminate solution or whether it is added during the subsequent annealing phase. It can also be added to the washed filter dough.
- the sodium sulfate can also be introduced during the washing process, which is carried out for the purpose of lowering the pH, by completely or partially neutralizing the sodium hydroxide which is in the wash water, which is expediently conducted in countercurrent, with sulfuric acid.
- the amount of sodium sulfate introduced in this way is generally not sufficient to improve the properties of sodium aluminum silicate doughs and powders, and further addition of sodium sulfate is required. Because of the exact dosage of sodium sulfate, an additional addition is usually necessary.
- the particle size distribution was carried out after dispersing in water (10 g of product; 700 ml of H 2 O; 60 min. Stirring at 1000 rpm) according to the Andreasen method.
- Example 2 In another part of the dough produced according to Example 1, after washing, 10 g of solid Na 2 SO 4 , corresponding to 2.4% of the amount of solids present in the dough, were mixed in per 1 kg of dough. The dough was also placed in a 200 liter jar to a filling height of 60 cm and observed as in Example 1. The simple tests, slowly tilting the container 45 °, inserting the stick, showed that after 7 days the dough was still homogeneous. After that, the phenomena that began to appear in a dough without Na 2 S0 4 addition began to appear.
- Example 1 In a further part of the dough produced according to Example 1, 100 g of solid Na 2 SO 4 were mixed in per 1 kg of dough, which corresponded to approximately 20% of the total amount of solids. The dough was observed when stored in the 200 liter jar with a filling height of 60 cm. In terms of flowability, the dough showed the same behavior as that in Example 3.
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Detergent Compositions (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE2738085 | 1977-08-24 | ||
| DE19772738085 DE2738085A1 (de) | 1977-08-24 | 1977-08-24 | Verfahren zur verbesserung der eigenschaften von natriumaluminiumsilikatteigen und -pulvern |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| EP0000870A1 true EP0000870A1 (fr) | 1979-03-07 |
Family
ID=6017132
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP78100496A Withdrawn EP0000870A1 (fr) | 1977-08-24 | 1978-07-25 | Procédé d'amélioration des propriétés des pâtes et poudres d'aluminosilicate de sodium |
Country Status (6)
| Country | Link |
|---|---|
| EP (1) | EP0000870A1 (fr) |
| AT (1) | ATA615178A (fr) |
| DE (1) | DE2738085A1 (fr) |
| DK (1) | DK371378A (fr) |
| IT (1) | IT1098273B (fr) |
| NO (1) | NO782864L (fr) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2488587A1 (fr) * | 1980-08-12 | 1982-02-19 | Toyo Soda Mfg Co Ltd | Zeolite en poudre a qualite elevee d'ecoulement, procede pour la preparer et composition detergente la contenant |
| EP0097512A3 (en) * | 1982-06-21 | 1986-02-26 | Unilever Plc | Aluminosilicates |
| FR2573769A1 (fr) * | 1984-11-26 | 1986-05-30 | Colgate Palmolive Co | Agglomerats bentonite-sulfate de sodium assouplissant les tissus, compositions detergentes les contenant, procede de fabrication des agglomerats et procede de lavage les utilisant |
| EP0279040A1 (fr) * | 1987-01-30 | 1988-08-24 | Degussa Aktiengesellschaft | Adjuvant actif pour agents de lavage |
| US5174918A (en) * | 1987-06-06 | 1992-12-29 | Degussa Ag | Stable aqueous suspensions of detergent zeolites and four oxo-alcohol ethoxylates |
| US5236680A (en) * | 1987-01-20 | 1993-08-17 | Mizusawa Industrial Chemicals, Ltd. | Preparation of amorphous silica-alumina particles by acid-treating spherical P-type zeolite particles crystallized from a sodium aluminosilicate gel |
| CN100411983C (zh) * | 2006-08-23 | 2008-08-20 | 中国铝业股份有限公司 | 超细硅酸铝的制备方法 |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2306167A1 (fr) * | 1975-04-02 | 1976-10-29 | Degussa | Procede de preparation de silicates d'aluminium |
| FR2319577A1 (fr) * | 1975-07-26 | 1977-02-25 | Henkel & Cie Gmbh | Procede de preparation d'aluminosilicates alcalins zeolitiques |
| FR2332321A1 (fr) * | 1975-11-18 | 1977-06-17 | Mizusawa Industrial Chem | Adjuvants pour detergents et procede pour leur preparation |
| FR2340128A1 (fr) * | 1976-02-06 | 1977-09-02 | Henkel & Cie Gmbh | Procede de preparation de suspensions aqueuses de silicates insolubles en fines particules echangeurs de cations, produits obtenus et leur utilisation pour la fabrication de produits de lavage et de nettoyage |
-
1977
- 1977-08-24 DE DE19772738085 patent/DE2738085A1/de not_active Withdrawn
-
1978
- 1978-07-25 EP EP78100496A patent/EP0000870A1/fr not_active Withdrawn
- 1978-08-22 IT IT26914/78A patent/IT1098273B/it active
- 1978-08-23 DK DK371378A patent/DK371378A/da unknown
- 1978-08-23 AT AT615178A patent/ATA615178A/de not_active Application Discontinuation
- 1978-08-23 NO NO782864A patent/NO782864L/no unknown
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2306167A1 (fr) * | 1975-04-02 | 1976-10-29 | Degussa | Procede de preparation de silicates d'aluminium |
| FR2319577A1 (fr) * | 1975-07-26 | 1977-02-25 | Henkel & Cie Gmbh | Procede de preparation d'aluminosilicates alcalins zeolitiques |
| FR2332321A1 (fr) * | 1975-11-18 | 1977-06-17 | Mizusawa Industrial Chem | Adjuvants pour detergents et procede pour leur preparation |
| FR2340128A1 (fr) * | 1976-02-06 | 1977-09-02 | Henkel & Cie Gmbh | Procede de preparation de suspensions aqueuses de silicates insolubles en fines particules echangeurs de cations, produits obtenus et leur utilisation pour la fabrication de produits de lavage et de nettoyage |
Non-Patent Citations (1)
| Title |
|---|
| CHEMICAL ABSTRACTS, vol. 78, 1973, no. 10, 12 maart, ref. 63318r, FRIEDRICH WOLF: "Hydrothermal synthesis of zeolitic molecular sieves in the presence of salts", page 334; & Z. Chem. 1972, 12(11), 422-3 (Ger.) * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2488587A1 (fr) * | 1980-08-12 | 1982-02-19 | Toyo Soda Mfg Co Ltd | Zeolite en poudre a qualite elevee d'ecoulement, procede pour la preparer et composition detergente la contenant |
| EP0097512A3 (en) * | 1982-06-21 | 1986-02-26 | Unilever Plc | Aluminosilicates |
| FR2573769A1 (fr) * | 1984-11-26 | 1986-05-30 | Colgate Palmolive Co | Agglomerats bentonite-sulfate de sodium assouplissant les tissus, compositions detergentes les contenant, procede de fabrication des agglomerats et procede de lavage les utilisant |
| US5236680A (en) * | 1987-01-20 | 1993-08-17 | Mizusawa Industrial Chemicals, Ltd. | Preparation of amorphous silica-alumina particles by acid-treating spherical P-type zeolite particles crystallized from a sodium aluminosilicate gel |
| EP0279040A1 (fr) * | 1987-01-30 | 1988-08-24 | Degussa Aktiengesellschaft | Adjuvant actif pour agents de lavage |
| US5174918A (en) * | 1987-06-06 | 1992-12-29 | Degussa Ag | Stable aqueous suspensions of detergent zeolites and four oxo-alcohol ethoxylates |
| CN100411983C (zh) * | 2006-08-23 | 2008-08-20 | 中国铝业股份有限公司 | 超细硅酸铝的制备方法 |
Also Published As
| Publication number | Publication date |
|---|---|
| ATA615178A (de) | 1980-08-15 |
| DK371378A (da) | 1979-02-25 |
| IT1098273B (it) | 1985-09-07 |
| IT7826914A0 (it) | 1978-08-22 |
| NO782864L (no) | 1979-02-27 |
| DE2738085A1 (de) | 1979-03-08 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PUAI | Public reference made under article 153(3) epc to a published international application that has entered the european phase |
Free format text: ORIGINAL CODE: 0009012 |
|
| AK | Designated contracting states |
Designated state(s): BE CH DE FR GB NL SE |
|
| STAA | Information on the status of an ep patent application or granted ep patent |
Free format text: STATUS: THE APPLICATION IS DEEMED TO BE WITHDRAWN |
|
| 18D | Application deemed to be withdrawn | ||
| RIN1 | Information on inventor provided before grant (corrected) |
Inventor name: WALTER, LUDWIG, DIPL.-CHEM. DR. Inventor name: RADEMACHER, THEO |