CN1101336C - Layered sodium disilicate and its preparation - Google Patents
Layered sodium disilicate and its preparation Download PDFInfo
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- CN1101336C CN1101336C CN01121390A CN01121390A CN1101336C CN 1101336 C CN1101336 C CN 1101336C CN 01121390 A CN01121390 A CN 01121390A CN 01121390 A CN01121390 A CN 01121390A CN 1101336 C CN1101336 C CN 1101336C
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- sodium disilicate
- layered sodium
- heteroatomic
- layered
- layer
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Abstract
The present invention relates to a layered sodium disilicate and a preparing method thereof, more specifically a layered sodium disilicate material as non-phosphate detergent and a preparing method thereof, which belongs to the field of inorganic application materials. The present invention is characterized in that hetero atoms are added in the synthesis of delta layered sodium disilicate, and hetero atom compounds are halogenide, oxide and sulfate of hetero atoms, so that the stability of the delta layered sodium disilicate in distilled water is effectively improved, and the delta layered sodium disilicate with high stability in distilled water is successfully prepared. The difficult problem is solved that delta layered sodium disilicate can not be used in proportioning before detergent production. The present invention has certain economical and social benefits.
Description
Layered sodium disilicate of the present invention and preparation belong to inorganic Material Used field, are specifically related to a kind of layered sodium disilicate material and preparation as the free phosphate detergent auxiliary agent.
Synthetic detergent is the requisite of human daily life, and in the preparation of synthetic detergent, the detergent builder that must add 15-20% improve the service efficiency of tensio-active agent to remove calcium, the magnesium ion in the water effectively.At present, the auxiliary agent that is most widely used is a tripoly phosphate sodium STPP, but its use has tangible pollution to environment, is one of primary pollution source of body eutrophication.
The no phosphatization of washing composition is the important content of environment protection.At present, the free phosphate detergent auxiliary agent that substitutes tripoly phosphate sodium STPP has: multiple materials such as 4A zeolite molecular sieve, hydrated sodium metasilicate, layered silicate, nitrilotriacetic acid, Trisodium Citrate, wherein layered sodium disilicate is that the end of the eighties is by the German Hoechst exploitation (U.S.Pat.No4 of company, 585,642, U.S.Pat.No4,820,439), its major advantage is environmental friendliness, calcium, the magnesium ion exchange capacity is big, surge capability strong, raw material is easy to get, production technique is simple.Comprehensively compare from aspects such as use properties and production costs, layered sodium disilicate is better than present widely used free phosphate detergent assistant 4 A zeolite molecular sieve, is a kind of ideal free phosphate detergent auxiliary agent.
The high tower desiccating method of dusting is mainly adopted in washing powder production at present.Before spraying drying, various raw materials need ground and mixed in 60-80 ℃ hot distilled water (needing 15-25 minute), in this process, require the various part maintain propertys that help stable.But in use find (U.S.Pat.No4,950,310): (65 ℃ of δ-layered sodium disilicate and hot distilled waters, 30 minutes) mix after, crystalline structure changes, product is converted into calcium, product that the magnesium ion exchange capacity is lower, has lost original performance, has had a strong impact on its use in preparing burden before washing composition is produced.
The purpose of layered sodium disilicate of the present invention and preparation is to solving the problem of above-mentioned existence, will introduce heteroatoms in δ-layered sodium disilicate synthetic, improves its stability in distilled water effectively.Thereby a kind of new modified δ-layered sodium disilicate material and preparation method thereof is provided, successfully prepares the δ-layered sodium disilicate of high stability in distilled water.
Layered sodium disilicate of the present invention is characterized in that it being a kind of two-dimensional layer crystalline structure with queueing discipline, in the crystalline structure of lamina sodium silicate, and two SiO
4The shared Sauerstoffatom of tetrahedron is connected to form electronegative layer each other, the layer with layer between be connected by the more weak positively charged ion of interaction force.δ-layered sodium disilicate has big port size, approaches circle, so δ-layered sodium disilicate has calcium, magnesium ion switching performance preferably.
The preparation of layered sodium disilicate of the present invention is characterized in that, will be at introducing heteroatoms in δ-layered sodium disilicate synthetic, and its described heteroatomic compound is heteroatomic halides, oxide compound and vitriol, refers to LiCl, KCl, MgCl
2, CaCl
2, FeCl
3, ZrOCl
2, AlCl
3, NaAlO
2, CaO, MgO, LiOH, K
2O, K
2SO
4, MgSO
4, Al
2(SO
4)
3
Synthetic the following these steps to that contains heteroatomic δ-layered sodium disilicate of the present invention carried out:
1. nickel crucible is placed in the dilute alkaline soln, soaked 24 hours down, take out, clean, dry at 100 ℃.
2. in nickel crucible, add a certain amount of heteroatomic compound (accounting for the 0.1%-5% of solid product total amount) that contains earlier, add liquid soluble glass 10ml then and stir, enter the retort furnace roasting.Maturing temperature is at 550-780 ℃, and roasting time is at 10min-180min.
Of the present inventionly contain heteroatomic δ-layered sodium disilicate stability test and follow these steps to carry out:
With layered sodium disilicate and the distilled water mixed with 1: 1, after stirring, airtight water bath with thermostatic control of putting into 80 ℃ is taken out rapidly to setting-up time, in 400 ℃ muffle furnace after the rapid drying, with the relative crystallinity of XRD test sample.
The measuring method of the calcium ion-exchanged capacity that contains heteroatomic δ-layered sodium disilicate of the present invention is as follows:
Pipette 50ml 0.05mol/lCaCl
2Solution is constant volume in the volumetric flask of 500ml, pours in the there-necked flask of 1000ml, drips 0.5mol/lNaOH solution the pH value is transferred to about 10.With there-necked flask constant temperature to 35 ± 1 ℃ in 35 ℃ water bath with thermostatic control, add load weighted sample 0.5g then, constant temperature filters after 20 minutes immediately under constantly stirring.The pipette, extract filtrate 50ml that uses 50ml then adds 2.5mol/lNaOH solution 2ml and a little calconcarboxylic acid in the 250ml Erlenmeyer flask, extremely become blue look by burgundy with the EDTA solution titration of 0.01mol/l.Method of calculation are as follows:
E＝100.08×(50×C
0-10×C
1×V
E)/m
Wherein:
C
0: CaCl
2The concentration of standardized solution, mol/l;
C
1: the concentration of EDTA standardized solution, mol/l;
V
E: consume the volume of EDTA standardized solution, ml;
M: the quality of sample, g.
The present invention contains heteroatomic δ-layered sodium disilicate and has following characteristics:
1. raw material is easy to get, and production cost is low, and preparation technology is simple.Adopt water glass and heteroatomic compound directly to mix, the method by roasting obtains product.
2. in delta-phase laminated sodium disilicate synthetic, behind the doping heteroatoms, can obtain the higher delta-phase laminated sodium disilicate of purity.
3. this product still has calcium and magnesium ion exchange capacity preferably; Surge capability is strong; With other detergent component good consistency is arranged.
4. this product can improve its stability in distilled water effectively on the basis of the original use properties of basic maintenance.
Embodiment 1:
Get the lithium chloride of 2 milliliters of 1mol/l and 10 ml water glass in nickel crucible, mix, place retort furnace to be heated to 700 ℃, constant temperature took out after 50 minutes.Product and distilled water is even by 1: 1 mixed, and mixture was placed 90 minutes down at 80 ℃, and is dry under 400 ℃, detects crystalline structure with XRD.The results are shown in Table 1
Embodiment 2:
Get the magnesium chloride of 2.5 milliliters of 1mol/l and 10 ml water glass in nickel crucible, mix, place retort furnace to be heated to 720 ℃, constant temperature took out after 35 minutes.Product and distilled water is even by 1: 1 mixed, and mixture was placed 90 minutes down at 80 ℃, and is dry under 400 ℃, detects crystalline structure with XRD.The results are shown in Table 1
Embodiment 3:
Get the aluminum chloride of 3 milliliters of 1mol/l and 10 ml water glass in nickel crucible, mix, place retort furnace to be heated to 730 ℃, constant temperature took out after 30 minutes.Product and distilled water is even by 1: 1 mixed, and mixture was placed 90 minutes down at 80 ℃, and is dry under 400 ℃, detects crystalline structure with XRD.The results are shown in Table 1
Embodiment 4:
Get the potassium oxide of 1.5 milliliters of 1mol/l and 10 ml water glass in nickel crucible, mix, place retort furnace to be heated to 750 ℃, constant temperature took out after 20 minutes.Product and distilled water is even by 1: 1 mixed, and mixture was placed 90 minutes down at 80 ℃, and is dry under 400 ℃, detects crystalline structure with XRD.The results are shown in Table 1
Embodiment 5:
Get the sodium metaaluminate of 1 milliliter of 1mol/l and 10 ml water glass in nickel crucible, mix, place retort furnace to be heated to 700 ℃, constant temperature took out after 50 minutes.Product and distilled water is even by 1: 1 mixed, and mixture was placed 90 minutes down at 80 ℃, and is dry under 400 ℃, detects crystalline structure with XRD.The results are shown in Table 1
Embodiment 6:
Get the lithium hydroxide of 0.8 milliliter of 1mol/l and 10 ml water glass in nickel crucible, mix, place retort furnace to be heated to 720 ℃, constant temperature took out after 30 minutes.Product and distilled water is even by 1: 1 mixed, and mixture was placed 90 minutes down at 80 ℃, and is dry under 400 ℃, detects crystalline structure with XRD.The results are shown in Table 1
Embodiment 7:
Get the vitriolate of tartar of 2.5 milliliters of 1mol/l and 10 ml water glass in nickel crucible, mix, place retort furnace to be heated to 760 ℃, constant temperature took out after 10 minutes.Product and distilled water is even by 1: 1 mixed, and mixture was placed 90 minutes down at 80 ℃, and is dry under 400 ℃, detects crystalline structure with XRD.The results are shown in Table 1
Embodiment 8
Get the Tai-Ace S 150 of 3 milliliters of 1mol/l and 10 ml water glass in nickel crucible, mix, place retort furnace to be heated to 780 ℃, promptly get to temperature.Product and distilled water is even by 1: 1 mixed, and mixture was placed 90 minutes down at 80 ℃, and is dry under 400 ℃, detects crystalline structure with XRD.The results are shown in Table 1
Ca after the preceding water logging of the experimental result sequence number hotchpotch temperature of reaction constant temperature time water logging of delta-phase laminated sodium disilicate among the embodiment
2+Exchange capacity
(mol) (℃) (min) thing phase thing phase (mgCaCO
3/ g) 1 0.002LiCl, 700 50 δ δ, 302 2 0.0025MgCl, 720 35 δ δ, 290 3 0.003AlCl
3730 30 δ δ, 293 4 0.0015K
2O 750 20 δ δ 298 5 0.001NaAlO
2700 50 δ δ, 289 6 0.0008LiOH, 720 30 δ δ, 300 7 0.0025K
2SO
4760 10 δ δ, 280 8 0.003Al
2(SO
4)
3780 0 δ δ 278
Claims (2)
1, layered sodium disilicate is characterized in that being a kind of two-dimensional layer crystalline structure with queueing discipline, in the crystalline structure of lamina sodium silicate, and two SiO
4The shared Sauerstoffatom of tetrahedron is connected to form electronegative layer each other, the layer with layer between be connected by the more weak positively charged ion of interaction force, δ-layered sodium disilicate has big port size, approaches circle.
2, according to the preparation of the described layered sodium disilicate of claim 1, it is characterized in that, will be at introducing heteroatoms in δ-layered sodium disilicate synthetic, its heteroatomic compound is heteroatomic halides, oxide compound and vitriol, refers to LiCl, KCl, MgCl
2, CaCl
2, FeCl
3, ZrOCl
2, AlCl
3, NaAlO
2, CaO, MgO, LiOH, K
2O, K
2SO
4, MgSO
4, Al
2(SO
4)
3,
Its synthetic following these steps to that contains heteroatomic δ-layered sodium disilicate is carried out:
At first nickel crucible is placed in the dilute alkaline soln, soaked 24 hours down at 100 ℃, take out, clean, dry, in nickel crucible, add a certain amount of heteroatomic compound that contains then, its content accounts for the 0.1%-5% of solid product total amount, then adds liquid soluble glass 10ml and stirs, and enters the retort furnace roasting, maturing temperature is at 550-780 ℃, and roasting time is at 10min-180min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN01121390A CN1101336C (en) | 2001-06-11 | 2001-06-11 | Layered sodium disilicate and its preparation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN01121390A CN1101336C (en) | 2001-06-11 | 2001-06-11 | Layered sodium disilicate and its preparation |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1322674A CN1322674A (en) | 2001-11-21 |
| CN1101336C true CN1101336C (en) | 2003-02-12 |
Family
ID=4664461
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN01121390A Expired - Fee Related CN1101336C (en) | 2001-06-11 | 2001-06-11 | Layered sodium disilicate and its preparation |
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| Country | Link |
|---|---|
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1088547A (en) * | 1991-12-21 | 1994-06-29 | 赫彻斯特股份公司 | The crystalline sodium disilicate preparation method |
| CN1157261A (en) * | 1995-10-12 | 1997-08-20 | 赫彻斯特股份公司 | Process for preparing sodium disilicate having high ion-exchange capacity |
| CN1262664A (en) * | 1997-07-16 | 2000-08-09 | 韩国化学研究所 | Process for preparation of crystalline layered sodium disilicate |
-
2001
- 2001-06-11 CN CN01121390A patent/CN1101336C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1088547A (en) * | 1991-12-21 | 1994-06-29 | 赫彻斯特股份公司 | The crystalline sodium disilicate preparation method |
| CN1157261A (en) * | 1995-10-12 | 1997-08-20 | 赫彻斯特股份公司 | Process for preparing sodium disilicate having high ion-exchange capacity |
| CN1262664A (en) * | 1997-07-16 | 2000-08-09 | 韩国化学研究所 | Process for preparation of crystalline layered sodium disilicate |
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| Publication number | Publication date |
|---|---|
| CN1322674A (en) | 2001-11-21 |
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