CN107445171B - A kind of preparation method of low index of refraction high transparency type silica - Google Patents
A kind of preparation method of low index of refraction high transparency type silica Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
- A61K8/25—Silicon; Compounds thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q11/00—Preparations for care of the teeth, of the oral cavity or of dentures; Dentifrices, e.g. toothpastes; Mouth rinses
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- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/20—Chemical, physico-chemical or functional or structural properties of the composition as a whole
- A61K2800/26—Optical properties
- A61K2800/262—Transparent; Translucent
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
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Abstract
The invention belongs to silica technical fields, and in particular to a kind of preparation method of low index of refraction high transparency type silica.Preparation method of the present invention includes S1 and prepares water glass solution, stands heat preservation, obtains waterglass colloidal sol crystal seed；S2, water intaking glass colloidal sol crystal seed, are diluted with water and prepare waterglass bottom liquid；S3 adds in waterglass bottom liquid and metabisulfite solution into reaction kettle, stirs evenly and heats；Waterglass colloidal sol crystal seed and sulfuric acid solution is added dropwise in S4 simultaneously, controls process pH, treats that waterglass colloidal sol crystal seed adds, and continues that sulfuric acid solution pH to terminal is added dropwise；S5 stops stirring, holding temperature, and the precipitation of silica of formation is carried out press filtration, washing by ageing, and silica is made in dry, crushing.Preparation method of the present invention is simple, and process stabilizing, production cost is low, and pollution is few, and silica obtained transparency under low index of refraction is high, applied to that in transparent toothpaste composition, can improve water consumption, wetting agent dosage is reduced, so as to reduce production cost.
Description
Technical field
The invention belongs to silica technical fields, and in particular to a kind of preparation of low index of refraction high transparency type silica
Method.
Background technology
In recent years, transparent toothpaste has become dental care products familiar to people.At present, silica is that manufacture is saturating
The indispensable raw material of bright toothpaste, chemical stability is good, good with multiple additives compatibility so that silica toothpaste is in market
On increasingly have competitiveness.
Make transparent toothpaste, it is necessary to the liquid-phase system of lotion and the index of refraction of solid system be made to be close, even up to
It is consistent.The main component of toothpaste liquid-phase system be water and wetting agent, and sorbierite, polyethylene glycol and glycerine belong to it is common
Wetting agent.In general, silica index of refraction is in the range of 1.4300~1.4600, and 70% sorbierite index of refraction is
1.457, the index of refraction of water is 1.333, and the index of refraction of polyethylene glycol is 1.46, and the index of refraction of glycerine is 1.47.70% sorbierite:
Water=90:10 solution index of refraction is 1.4458,70% sorbierite:Water=87.5:12.5 solution index of refraction is 1.4390,
70% sorbierite:Water=85:15 solution index of refraction is 1.4340,70% sorbierite:Water=80:20 solution index of refraction is
1.4300.Make liquid phase consistent with the index of refraction of solid phase by the ratio for adjusting wetting agent and water, so as to reach transparent effect.Except
Beyond index of refraction, the transparency of silica is also extremely important, and general requirement is more than 85%.As long as two more than being provided simultaneously with
Condition would not generate diffusing reflection, so as to form the preferable lotion of transparency.
At present, silica in the transparency of 1.4400~1.4600 scope of index of refraction up to more than 90%, but low
The transparency of 1.4300~1.4400 scope of index of refraction is then less than 80%.In transparent toothpaste composition, water consumption is all often very
Few, general 10% or so, and the dosage of wetting agent such as sorbierite, polyethylene glycol or glycerine is more than 70%, it is seen that transparent tooth
The height of the cost of manufacture of cream.Therefore, it is necessary to a kind of preparation method of silica is researched and developed, to prepare low index of refraction high transparency
The silica of type is applied in transparent toothpaste composition, can improve water consumption, reduces wetting agent dosage, so as to reduce production
Cost.
The content of the invention
In order to solve the problems, such as present in existing Silica Using for Toothpaste that transparency is low under low index of refraction, the present invention carries
Supplied a kind of preparation method of low index of refraction high transparency type silica, can improve silica low index of refraction 1.4300~
The transparency of 1.4400 scopes reaches more than 85%, and is maintained at the transparency of 1.4400~1.4600 scope of index of refraction
More than 90%.
The preparation method of low index of refraction high transparency type silica provided by the invention, specifically includes following steps：
S1, the water glass solution that compound concentration is 2.0~3.0M, 8~12h of heat preservation is stood at 30~50 DEG C, obtains water glass
Glass colloidal sol crystal seed；
S2, water intaking glass colloidal sol crystal seed, are diluted with water, and compound concentration is the waterglass bottom liquid of 0.5~1.0M；
S3, waterglass bottom 3~5m of liquid is added in into reaction kettle3With 10~15m of metabisulfite solution3, stir evenly and be heated to
55~75 DEG C；
S4 while 10~15m of waterglass colloidal sol crystal seed is added dropwise3And sulfuric acid solution, it is 7~9 to control process pH, treats waterglass
Colloidal sol crystal seed is added dropwise, and continuing dropwise addition sulfuric acid solution, pH is 5.0~6.0 to terminal, stirs 30~50min；
S5, stop stirring, kept for 55~75 DEG C, the precipitation of silica of formation is carried out press filtration, washing, to washing by ageing
Silica after washing is dried, crushes, and low index of refraction high transparency type silica is made.
Further, the concentration of the metabisulfite solution is 5.0~10.0%.
Further, the concentration of the sulfuric acid solution is 5.0~8.0M.
Further, it is 7~8 that process pH is controlled in the step S4.
Further, sulfuric acid solution is added dropwise in the step S4, and pH is 5.4~5.8 to terminal.
Further, the time being aged in the step S5 is 1~2h.
In the technical solution of the present invention, waterglass is used as reaction raw materials, using sodium sulphate as reaction promoter, is carried out with sulfuric acid
Neutralization reaction controls the parameters such as concentration, temperature, pH value in reaction process, high transparency type silica under low index of refraction is made.
Using the waterglass of two concentration gradients in the preparation method of the present invention, with low concentration waterglass and salting-out agents sulphur
Acid sodium solution is as bottom liquid, when higher concentration waterglass and sulfuric acid solution react, on the one hand using salting-out agents metabisulfite solution as
Reaction promoter destroys the stability of waterglass and the silicon dioxide gel of sulfuric acid reaction generation and is settled out silica, another
Aspect guides higher concentration waterglass and sulfuric acid preferably hybrid reaction with low concentration waterglass, make reaction uniformly, it is steady
Ground carries out, and the precipitation of silica dioxide gel is avoided, so as to which the silica that transparency is high under low index of refraction be made.
In addition, waterglass is a kind of solution based on silicate particles, supplemented by colloidal particle, it is dual to be that one kind possesses
The dispersion of property, is atypical colloidal solution, and step S1 is quiet at 30~50 DEG C by the water glass solution of higher concentration
Put 8~12h of heat preservation, may be such that water glass solution reaches stable dispersity, with ensure ingredient it is uniform prevent aging, and
Inventor is but very beneficial for improving silica under low index of refraction it was unexpectedly observed that so simple heat preservation stewing process
Transparency.Step S3 strictly controls the dosage of salting-out agents metabisulfite solution, and silica can be influenced by adding in excessive sodium sulphate
The purity of product, so as to influence its transparency；It adds in very few sodium sulphate and then easily precipitates insufficient, cause the appearance of gel,
The transparency of silica product can equally be caused to decline.Reaction process also needs strict temperature control as 55~75 DEG C, reaction temperature
Spend low, then reaction process has gel appearance, and reaction temperature is excessively high, then product transparency declines.Therefore, each step phase of the present invention
It is auxiliary to coordinate, the silica that transparency is high under low index of refraction is made, the silica is in 1.4300~1.4400 model of index of refraction
The transparency enclosed is maintained at more than 90% up to more than 85%, in the transparency of 1.4400~1.4600 scope of index of refraction.
Therefore, compared with prior art, advantage of the invention is that：
(1) preparation method of the present invention can improve transparency of the silica in low 1.4300~1.4400 scope of index of refraction,
More than 85% is reached, and the transparency for being maintained at 1.4400~1.4600 scope of index of refraction is made more than 90%
Silica be applied in transparent toothpaste, can improve water consumption, reduce wetting agent dosage, so as to reduce production cost, improve
Economic benefit.
(2) preparation method of the present invention is simple, and process stabilizing, condition is controllable, and production cost is low, low in the pollution of the environment, can industry
Metaplasia is produced.
Specific embodiment
Below in conjunction with specific embodiment, the present invention will be described in detail, herein illustrative examples and explanation of the invention
For explaining the present invention, but it is not as a limitation of the invention.
The preparation method of embodiment 1, the low index of refraction high transparency type silica of the present invention
S1, the water glass solution that compound concentration is 2.0M, heat preservation 12h is stood at 30 DEG C, obtains waterglass colloidal sol crystal seed；
S2, water intaking glass colloidal sol crystal seed, are diluted with water, and compound concentration is the waterglass bottom liquid of 0.5M；
S3, waterglass bottom liquid 3m is added in into reaction kettle3With the metabisulfite solution 10m that concentration is 5.0%3, stir evenly simultaneously
It is heated to 55 DEG C；
S4 while waterglass colloidal sol crystal seed 10m is added dropwise3With the sulfuric acid solution that concentration is 5.0M, it is 7~8 to control process pH,
Treat that waterglass colloidal sol crystal seed is added dropwise, continuing dropwise addition sulfuric acid solution, pH is 5.0~5.5 to terminal, stirs 30min；
S5, stop stirring, kept for 55 DEG C, be aged 1h, the precipitation of silica of formation is subjected to press filtration, washing, to washing
Silica afterwards is dried, crushes, and low index of refraction high transparency type silica is made.
The preparation method of embodiment 2, the low index of refraction high transparency type silica of the present invention
S1, the water glass solution that compound concentration is 3.0M, heat preservation 8h is stood at 50 DEG C, obtains waterglass colloidal sol crystal seed；
S2, water intaking glass colloidal sol crystal seed, are diluted with water, and compound concentration is the waterglass bottom liquid of 1.0M；
S3, waterglass bottom liquid 5m is added in into reaction kettle3With the metabisulfite solution 15m that concentration is 10.0%3, stir evenly
And it is heated to 75 DEG C；
S4 while waterglass colloidal sol crystal seed 15m is added dropwise3With the sulfuric acid solution that concentration is 8.0M, it is 8~9 to control process pH,
Treat that waterglass colloidal sol crystal seed is added dropwise, continuing dropwise addition sulfuric acid solution, pH is 5.5~6.0 to terminal, stirs 50min；
S5, stop stirring, kept for 75 DEG C, be aged 2h, the precipitation of silica of formation is subjected to press filtration, washing, to washing
Silica afterwards is dried, crushes, and low index of refraction high transparency type silica is made.
The preparation method of embodiment 3, the low index of refraction high transparency type silica of the present invention
S1, the water glass solution that compound concentration is 3.0M, heat preservation 10h is stood at 40 DEG C, obtains waterglass colloidal sol crystal seed；
S2, water intaking glass colloidal sol crystal seed, are diluted with water, and compound concentration is the waterglass bottom liquid of 0.5M；
S3, waterglass bottom liquid 4m is added in into reaction kettle3With the metabisulfite solution 12m that concentration is 8.0%3, stir evenly simultaneously
It is heated to 65 DEG C；
S4 while waterglass colloidal sol crystal seed 13m is added dropwise3With the sulfuric acid solution that concentration is 6.0M, it is 7~8 to control process pH,
Treat that waterglass colloidal sol crystal seed is added dropwise, continuing dropwise addition sulfuric acid solution, pH is 5.4~5.8 to terminal, stirs 40min；
S5, stop stirring, kept for 65 DEG C, be aged 2h, the precipitation of silica of formation is subjected to press filtration, washing, to washing
Silica afterwards is dried, crushes, and low index of refraction high transparency type silica is made.
The preparation method of embodiment 4, the low index of refraction high transparency type silica of the present invention
S1, the water glass solution that compound concentration is 2.0M, heat preservation 10h is stood at 30 DEG C, obtains waterglass colloidal sol crystal seed；
S2, water intaking glass colloidal sol crystal seed, are diluted with water, and compound concentration is the waterglass bottom liquid of 1.0M；
S3, waterglass bottom liquid 4m is added in into reaction kettle3With the metabisulfite solution 14m that concentration is 7.0%3, stir evenly simultaneously
It is heated to 65 DEG C；
S4 while waterglass colloidal sol crystal seed 12m is added dropwise3With the sulfuric acid solution that concentration is 7.0M, it is 8~9 to control process pH,
Treat that waterglass colloidal sol crystal seed is added dropwise, continuing dropwise addition sulfuric acid solution, pH is 5.4~5.8 to terminal, stirs 40min；
S5, stop stirring, kept for 65 DEG C, be aged 1h, the precipitation of silica of formation is subjected to press filtration, washing, to washing
Silica afterwards is dried, crushes, and low index of refraction high transparency type silica is made.
The preparation method of embodiment 5, the low index of refraction high transparency type silica of the present invention
S1, the water glass solution that compound concentration is 3.0M, heat preservation 10h is stood at 40 DEG C, obtains waterglass colloidal sol crystal seed；
S2, water intaking glass colloidal sol crystal seed, are diluted with water, and compound concentration is the waterglass bottom liquid of 1.0M；
S3, waterglass bottom liquid 4m is added in into reaction kettle3With the metabisulfite solution 12m that concentration is 8.0%3, stir evenly simultaneously
It is heated to 65 DEG C；
S4 while waterglass colloidal sol crystal seed 12m is added dropwise3With the sulfuric acid solution that concentration is 6.0M, it is 7~8 to control process pH,
Treat that waterglass colloidal sol crystal seed is added dropwise, continuing dropwise addition sulfuric acid solution, pH is 5.4~5.8 to terminal, stirs 30min；
S5, stop stirring, kept for 65 DEG C, be aged 1h, the precipitation of silica of formation is subjected to press filtration, washing, to washing
Silica afterwards is dried, crushes, and low index of refraction high transparency type silica is made.
Comparative example 1
S1, respectively compound concentration are the water glass solution of 3.0M and 1.0M；
S2, the water glass solution 4m that concentration is 1.0M is added in into reaction kettle3With the metabisulfite solution that concentration is 8.0%
12m3, stir evenly and be heated to 65 DEG C；
S3 at the same be added dropwise concentration be 3.0M water glass solution 12m3Sulfuric acid solution with concentration is 6.0M, controls process
PH is 7~8, treats that water glass solution is added dropwise, and continuing dropwise addition sulfuric acid solution, pH is 5.4~5.8 to terminal, stirs 30min；
S4, stop stirring, kept for 65 DEG C, be aged 1h, the precipitation of silica of formation is subjected to press filtration, washing, to washing
Silica afterwards is dried, crushes, and low index of refraction high transparency type silica is made.
Comparative example 2
Compared with Example 5, this comparative example differs only in：The addition of metabisulfite solution is 8m3.As a result in step
There are a large amount of gels to generate in the reaction process of S4.
Comparative example 3
Compared with Example 5, this comparative example differs only in：The addition of metabisulfite solution is 16m3。
Comparative example 4
Compared with Example 5, this comparative example differs only in：50 DEG C, i.e. controlling reaction temperature are heated in step S2
For 50 DEG C.As a result a large amount of gels generate in the reaction process of step S4.
Comparative example 5
Compared with Example 5, this comparative example differs only in：80 DEG C, i.e. controlling reaction temperature are heated in step S2
For 80 DEG C.
Test example
To silica made from the embodiment of the present invention 1~5, comparative example 1~5 in 1.4300~1.4600 scope of index of refraction
Transparency be detected, the result is shown in the following table 1.
The testing result table of 1 each silica of table transparency under different indexs of refraction
Seen from table 1 above, the silica prepared by the embodiment of the present invention 1~5 is in 1.4300~1.4400 model of index of refraction
The transparency enclosed is maintained at more than 90% up to more than 85%, in the transparency of 1.4400~1.4600 scope of index of refraction, by these
Silica is applied in the toothpaste that water content is 15%, and lotion transparent clear improves the water consumption in toothpaste, reduces profit
Humectant dosage, so as to reduce production cost.
Compared with the preparation method of the present invention, the water glass solution of comparative example 1 does not carry out standing isothermal holding, as a result institute
The transparency for the silica produced declines；Comparative example 2 and comparative example 3 reduce and add respectively the dosage of sodium sulphate, as a result
There are a large amount of gels to generate in the preparation process of comparative example 2, and the transparency of silica obtained is decreased obviously, and comparative example
The transparency of 3 silica produced equally declines apparent；Comparative example 4 and comparative example 5, which are reduced and improved respectively, reacted
The temperature of journey, the transparency of as a result obtained silica are decreased obviously, and are also had in the preparation process of comparative example 4 big
Gel is measured to generate；The above results illustrate that each parameter complements each other with step in preparation method of the present invention, low so as to be prepared
Index of refraction high transparency type silica.
The above-described embodiments merely illustrate the principles and effects of the present invention, and is not intended to limit the present invention.It is any ripe
Know the personage of this technology all can carry out modifications and changes under the spirit and scope without prejudice to the present invention to above-described embodiment.Cause
This, those of ordinary skill in the art is complete without departing from disclosed spirit and institute under technological thought such as
Into all equivalent modifications or change, should by the present invention claim be covered.
Claims (4)
1. a kind of preparation method of low index of refraction high transparency type silica, which is characterized in that comprise the following steps：
S1, the water glass solution that compound concentration is 2.0~3.0M, 8~12h of heat preservation is stood at 30~50 DEG C, it is molten to obtain waterglass
Glue crystal seed；
S2, water intaking glass colloidal sol crystal seed, are diluted with water, and compound concentration is the waterglass bottom liquid of 0.5~1.0M；
S3, waterglass bottom 3~5m3 of liquid and 10~15m3 of metabisulfite solution are added in into reaction kettle, stir evenly and is heated to 55
~75 DEG C；
S4 while waterglass 10~15m3 of colloidal sol crystal seed and sulfuric acid solution is added dropwise, process pH is controlled to treat waterglass colloidal sol for 7~9
Crystal seed is added dropwise, and continuing dropwise addition sulfuric acid solution, pH is 5.0~6.0 to terminal, stirs 30~50min；
S5, stop stirring, kept for 55~75 DEG C, the precipitation of silica of formation is carried out press filtration, washing, after washing by ageing
Silica be dried, crush, be made low index of refraction high transparency type silica；
The concentration of the metabisulfite solution is 5.0~10.0%；
The concentration of the sulfuric acid solution is 5.0~8.0M.
2. the preparation method of low index of refraction high transparency type silica as described in claim 1, which is characterized in that the step S4
It is middle to control process pH as 7~8.
3. the preparation method of low index of refraction high transparency type silica as described in claim 1, which is characterized in that the step S4
PH is 5.4~5.8 to middle dropwise addition sulfuric acid solution to terminal.
4. the preparation method of low index of refraction high transparency type silica as described in claim 1, which is characterized in that the step S5
The time of middle ageing is 1~2h.
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| CN110591416A (en) * | 2019-08-23 | 2019-12-20 | 广州凌玮科技股份有限公司 | Preparation method of amorphous silicon dioxide antirust pigment |
| CN112408406B (en) * | 2020-12-04 | 2021-08-06 | 广州市飞雪材料科技有限公司 | Low-refraction high-cleaning friction type silicon dioxide for toothpaste and preparation method thereof |
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