CN1239390C - High pure delta layered sodium disilicate and producing process thereof - Google Patents
High pure delta layered sodium disilicate and producing process thereof Download PDFInfo
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- CN1239390C CN1239390C CN 200410012441 CN200410012441A CN1239390C CN 1239390 C CN1239390 C CN 1239390C CN 200410012441 CN200410012441 CN 200410012441 CN 200410012441 A CN200410012441 A CN 200410012441A CN 1239390 C CN1239390 C CN 1239390C
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- sodium disilicate
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Abstract
The present invention relates to delta layered sodium disilicate with high purity and a preparing method thereof, more specifically layered sodium disilicate material used as an auxiliary agent and a preparing method thereof, which belongs to the field of inorganic utilization material. The present invention is characterized in that liquid water glass with the module of 2.06 to 2.25 is put in an environment with the high temperature of 700 to 750 DEG C to synthesize the delta layered sodium disilicate in a short time. The preparing method has the advantages of easy acquirement of raw material, low production cost and simple preparing technology. The layered sodium disilicate material has the advantages of favorable exchange capability of calcium ions and magnesium ions and strong buffering capability, and compared with other detergent constituents, the layered sodium disilicate material has favorable compatibility and certain economical and social benefits.
Description
One, technical field
The preparation method of high purity δ layered sodium disilicate of the present invention belongs to inorganic Material Used field, specifically relates to a kind of layered sodium disilicate preparation methods as auxiliary agent.
Two, technical background
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), they comprise α, β and δ layered sodium disilicate mutually.Their 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 ideal free phosphate detergent auxiliary agent.
At present, the mode of production of layered sodium disilicate mainly contains two kinds, a kind of is synthetic with the liquid soluble glass direct sintering, concrete method is: liquid soluble glass according to certain temperature rise rate, be heated to invert point (being generally 650-800 ℃), constant temperature 10-600 minute, (650-680 ℃ is produced β phase layered sodium disilicate was main product to synthetic layered sodium disilicate; 700-730 ℃ is produced delta-phase laminated sodium disilicate is main product; The 750-800 ℃ of layered sodium disilicate of producing the α phase is main product); Second method is, at first liquid soluble glass process spraying drying, be prepared into quick dissolved sodium silicate, the hot gas flow of quick dissolved sodium silicate with 650-750 ℃ heated 10-30 minute again, (650-700 ℃ is produced β phase layered sodium disilicate is main product to synthetic layered sodium disilicate; 700-750 ℃ is produced delta-phase laminated sodium disilicate is main product; The 750-800 ℃ of layered sodium disilicate of producing the α phase is main product).But the layered sodium disilicate purity that above-mentioned two kinds of methods are produced is all lower, and β phase layered sodium disilicate is main product, and the content of β phase is at 75-80%; Delta-phase laminated sodium disilicate is main product, and the δ phase content can reach 85-90%.But employing can industrialized production approach, and synthetic content surpasses 95% layered sodium disilicate product, remains a technical barrier that not have solution.
Three, summary of the invention
The preparation method of high purity δ layered sodium disilicate of the present invention, purpose are, solve the shortcoming that above-mentioned the whole bag of tricks exists, thereby disclose a kind of technical scheme of method of synthesis of high purity layered sodium disilicate.
The preparation method of high purity δ layered sodium disilicate of the present invention, it is characterized in that nickel, stainless steel alkali corrosion resistance crucible, sodium hydroxide solution with 5-30% concentration was handled 1-3 hour, and be washed with distilled water to neutrality, with modulus is that the liquid soluble glass of 2.06-2.25 places 700-750 ℃, and the content of synthetic δ phase reaches δ-layered sodium disilicate of 95-100% in 2-10 minute.
The preparation of above-mentioned synthetic δ-layered sodium disilicate follows these steps to carry out:
I. with the crucible of alkali corrosion resistances such as nickel, stainless steel, handled 1-3 hour with the sodium hydroxide solution of 5-30% concentration, and be washed with distilled water to neutrality.
II. the liquid soluble glass with metering places corrosion resistant container.
III. this container is placed in the retort furnace and is warmed up to suitable maturing temperature 700-750 ℃ according to certain speed, roasting time was at 2-10 minute.
High purity stratiform sodium disilicate synthesis method of the present invention has following characteristics:
1. raw material is easy to get, and production cost is low, and preparation technology is simple.Adopt liquid sodium silicate (being liquid soluble glass), obtain product by the method for roasting.
2. at the synthetic delta-phase laminated sodium disilicate of high temperature, can obtain purity and be higher than 95% product.
3. this product has calcium and magnesium ion exchange capacity preferably; Surge capability is strong; With other detergent component good consistency is arranged.
Four, embodiment
Embodiment 1:
With the crucible of stainless steel alkali corrosion resistance, handled 1 hour with the sodium hydroxide solution of 5% concentration, and be washed with distilled water to neutrality.Take by weighing 10 gram liquid sodium silicates (modulus 2.06) in the crucible of stainless steel alkali corrosion resistance, be warmed up to 700 ℃ in retort furnace, constant temperature took out after 2 minutes.Detect crystalline structure with XRD.The results are shown in Table.
Embodiment 2:
With the crucible of nickel alkali corrosion resistance, handled 2 hours with the sodium hydroxide solution of 25% concentration, and be washed with distilled water to neutrality.Take by weighing 10 gram liquid sodium silicates (modulus 2.15) in nickel crucible, be warmed up to 720 ℃ in retort furnace, constant temperature took out after 5 minutes.Detect crystalline structure with XRD.The results are shown in Table.
Embodiment 3:
With the crucible of nickel alkali corrosion resistance, handled 3 hours with the sodium hydroxide solution of 30% concentration, and be washed with distilled water to neutrality.Take by weighing 10 gram liquid sodium silicates (modulus 2.25) in nickel crucible, be warmed up to 750 ℃ in retort furnace, constant temperature took out after 2 minutes.Detect crystalline structure with XRD.The results are shown in Table.
Embodiment 4:
With the crucible of nickel alkali corrosion resistance, handled 3 hours with the sodium hydroxide solution of 10% concentration, and be washed with distilled water to neutrality.Take by weighing 10 gram liquid sodium silicates (modulus 2.25) in nickel crucible, be warmed up to 735 ℃ in retort furnace, constant temperature took out after 10 minutes.Detect crystalline structure with XRD.The results are shown in Table.
Embodiment 5:
With the crucible of stainless steel alkali corrosion resistance, handled 1 hour with the sodium hydroxide solution of 25% concentration, and be washed with distilled water to neutrality.Take by weighing 10 gram liquid sodium silicates (modulus 2.10) in Stainless Steel Crucible, be warmed up to 735 ℃ in retort furnace, constant temperature took out after 6 minutes.Detect crystalline structure with XRD.The results are shown in Table.
Embodiment 6:
With the crucible of stainless steel alkali corrosion resistance, handled 1.6 hours with the sodium hydroxide solution of 16% concentration, and be washed with distilled water to neutrality.Take by weighing 10 gram liquid sodium silicates (modulus 2.20) in Stainless Steel Crucible, be warmed up to 740 ℃ in retort furnace, constant temperature took out after 3 minutes.Detect crystalline structure with XRD.The results are shown in Table.
The experimental result table of delta-phase laminated sodium disilicate among the embodiment
| Sequence number | Temperature of reaction (℃) | Constant temperature time (seconds) | The thing phase | Ca 2+Exchange capacity (mgCaCO 3/g) |
| 1 2 3 4 5 6 | 700 720 750 750 735 740 | 120 300 120 600 360 190 | 95％δ+5％β 100％δ 98％δ+2％α 95％δ+5％α 99％δ+2％α 99％δ+2％β | 331 335 318 311 329 321 |
Claims (1)
1. the preparation method of a high purity δ layered sodium disilicate, it is characterized in that nickel, stainless steel alkali corrosion resistance crucible, sodium hydroxide solution with 5-30% concentration was handled 1-3 hour, and be washed with distilled water to neutrality, with modulus is that the liquid soluble glass of 2.06-2.25 places 700-750 ℃, and the content of synthetic δ phase reaches δ-layered sodium disilicate of 95-100% in 2-10 minute.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN 200410012441 CN1239390C (en) | 2004-07-23 | 2004-07-23 | High pure delta layered sodium disilicate and producing process thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410012441 CN1239390C (en) | 2004-07-23 | 2004-07-23 | High pure delta layered sodium disilicate and producing process thereof |
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| CN1576233A CN1576233A (en) | 2005-02-09 |
| CN1239390C true CN1239390C (en) | 2006-02-01 |
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| CN 200410012441 Expired - Fee Related CN1239390C (en) | 2004-07-23 | 2004-07-23 | High pure delta layered sodium disilicate and producing process thereof |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103193240A (en) * | 2013-05-02 | 2013-07-10 | 杨敏 | Production method of laminated sodium silicate based on delta phase |
| CN109794249B (en) * | 2019-01-25 | 2021-11-19 | 太原理工大学 | Preparation method of layered copper zinc silicate nanosheet |
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