CN105129806A - High-specific surface area silica for washing powder and its preparation method and use - Google Patents
High-specific surface area silica for washing powder and its preparation method and use Download PDFInfo
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- CN105129806A CN105129806A CN201510452397.2A CN201510452397A CN105129806A CN 105129806 A CN105129806 A CN 105129806A CN 201510452397 A CN201510452397 A CN 201510452397A CN 105129806 A CN105129806 A CN 105129806A
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Abstract
The invention discloses high-specific surface area silica for washing powder and its preparation method and use. The preparation method comprises S1, adding water into a reactor, carrying out heating to a temperature of 65-75 DEG C, adding glycerin into the water and carrying out stirring to obtain a uniform mixture, S2, adding sodium silicate and sulfuric acid into mixture together, stopping sulfuric acid addition when the system pH is in a range of 2.0-3.0 and carrying out ageing for 1.5-2.5h, and S3, carrying out filter pressing on the aged silicon dioxide, carrying out washing, carrying out drying and carrying out fragmentation to obtain the high-specific surface area silica for washing powder. The preparation method has simple processes, easily controllable conditions and a low production cost. The high-specific surface area silica has a uniform structure, a high-specific surface area of 600-700m<2>/g, a pore volume of 2.8-3.0cm<3>/g and pore sizes of 16-20nm and completely satisfies requirements on good use in washing powder.
Description
Technical field
The invention belongs to the technical field of precipitated silica, be specifically related to silicon-dioxide of a kind of washing powder high-specific surface area and preparation method thereof and the application in washing powder.
Background technology
In existing washing powder formula, tripoly phosphate sodium STPP is universally acknowledged detergent builder compound of good performance.But due to the body eutrophication problem that the rich phosphorus in phosphorus-containing detergent causes, cause environmental pollution, cause the low-phosphorous and without phosphorus topic changed into as current washing powder industry hot topic.Many industrially developed country all expressly provide and forbid producing and using phosphorous articles for washing.Therefore, people start to seek a kind of effective substitute to reduce the use even eliminating tripoly phosphate sodium STPP.
Silicon-dioxide prepared by the precipitator method has high-specific surface area, very high adsorptivity, very strong dispersiveness and good suspending power, and it can be used as a kind of washing assistant to be added in articles for washing is a kind of desirable selection.But for the silicon-dioxide in washing composition need possess high-specific surface area, large pore volume aperture could meet its application in washing composition, silicon-dioxide specific surface area, pore volume aperture prepared by the tradition precipitator method are also enough not large, its applications well in washing composition can not be met completely, the effect of high absorption, strong dispersion, well suspended can not be reached completely.
Chinese patent application CN104192851A discloses a kind of method preparing nano silicon, and the method step is as follows: (1) adds glycerine in sodium silicate solution, and the consumption of glycerine is the 2-5% of water glass quality; (2) in the mixed solution of step (1), add sulfuric acid, to pH=5-6, stir 1-2 hour, obtain nano silicon.This patent is compared with traditional precipitator method, and in precipitin reaction, add glycerine as crystal growth control agent, thus obtain the nanometer silicon dioxide particle of particle diameter 70-90nm, particle dispersion is high, and pattern is homogeneous; But this patent does not disclose the index such as specific surface area, pore volume of this nano silicon.
Chinese patent application CN102002120A discloses a kind of preparation method of large pore volume bigger serface special silica-gel carrier, the steps include: industrial metasilicate to dilute, at temperature 20-40 DEG C, drip inorganic acid solution, regulation system pH to 2-4, be warming up to 80-100 DEG C, add specific surface control agent; Specific surface control agent is selected from ethylene glycol, ethyl acetate, glycerol, acetone, one or more of trichloroethane, and insulation 2-4 hour, carries out hydro-thermal reaction; Then ageing 1-2 hour; Washing; Dry; Carry out size classification, obtain that pore volume is 2.5-2.8ml/g, specific surface area is 500-600m
2the silicon-dioxide of/g, but the specific surface area of this silicon-dioxide, pore volume etc. are also desirable not to the utmost, and this preparation method is consuming time, production cost is higher.
In sum, be necessary to research and develop the silicon-dioxide and preparation method thereof in a kind of high-specific surface area, large pore volume aperture, to meet its applications well in washing powder.
Summary of the invention
For the deficiency that current precipitated silica and preparation method thereof exists, the invention provides the silicon-dioxide that a kind of preparation method of washing powder high specific surface area silica and this preparation method obtain, solve silicon-dioxide that traditional precipitator method obtain and there is the little shortcoming in specific surface area, pore volume aperture, this preparation method is simple simultaneously, condition is controlled, and production cost is low.
The present invention is by the following technical programs to realize above-mentioned purpose: a kind of preparation method of washing powder high specific surface area silica, comprises the following steps:
S1, in retort, add water, be heated to 65 ~ 75 DEG C, then add glycerine, stir;
S2, add water glass and sulfuric acid simultaneously, stop when system pH is 2.0 ~ 3.0 adding sulfuric acid, ageing 1.5 ~ 2.5h;
S3, the silica batch after ageing carried out press filtration washing, dry broken, obtain washing powder high specific surface area silica.
Further, the weight ratio of described glycerine and water is (0.012 ~ 0.018): 1.
Further, the weight ratio of described glycerine and water is 0.018:1.
Further, the concentration of described water glass is 0.6 ~ 0.8mol/L, and the volume ratio of itself and water is (0.8 ~ 1.2): 1, and the flow velocity added is 13 ~ 16m
3/ h.Further, the concentration of described water glass is 0.7mol/L, and the volume ratio of itself and water is 1:1, and the flow velocity added is 15m
3/ h.
Further, the concentration of described sulfuric acid is 4 ~ 6mol/L, and the flow velocity added is 2.4 ~ 2.8m
3/ h.Further, the concentration of described sulfuric acid is 5mol/L, and the flow velocity added is 2.6m
3/ h.
In technique scheme, using water as mother liquor, first water is added and heat temperature raising in retort, then glycerine is added, glycerine is uniformly dispersed in the hot water, then water glass and sulfuric acid stream add simultaneously, being created in the solution environmental of a unusual stable homogeneous of silicon-dioxide is carried out, obtains homogeneous structural.The consumption of glycerine is and the weight ratio of water (0.012 ~ 0.018): 1, and this consumption can be good at the growth structure controlling silicon-dioxide, reaches the object improving pore volume aperture, specific surface area.Silicon-dioxide, 2.0 ~ 3.0, is carried out ageing and soaks the object reaching and expand pore volume aperture further by control of reaction end point in a sour environment.
The specific surface area of the silicon-dioxide that the preparation method of washing powder high specific surface area silica of the present invention obtains is 600 ~ 700m
2/ g, pore volume is 2.8 ~ 3.0cm
3/ g, aperture is 16 ~ 20nm, can meet its applications well in washing powder completely, reaches the effect of high absorption, strong dispersion, well suspended.
Therefore, compared with prior art, advantage of the present invention is:
Preparation method's technique of washing powder high specific surface area silica of the present invention is simple, and condition is easily controlled, and production cost is low, and obtained silicon dioxide structure is homogeneous, and specific surface area is 600 ~ 700m
2/ g, pore volume is 2.8 ~ 3.0cm
3/ g, aperture is 16 ~ 20nm, reaches the effect of high absorption, strong dispersion, well suspended, can be used as a kind of washing assistant, can meet its applications well in washing powder completely, remove the spot on clothing well.
Embodiment
Describe the present invention in detail below in conjunction with specific embodiment, be used for explaining the present invention in this illustrative examples of the present invention and explanation, but not as a limitation of the invention.
the preparation method of embodiment 1, washing powder high specific surface area silica of the present invention
S1, in retort, add 12m
3water, be heated to 70 DEG C, then add 216kg glycerine, stir;
S2, with 15m
3the flow velocity of/h adds the water glass 12m that concentration is 0.7mol/L
3, simultaneously with 2.6m
3it is 5mol/L sulfuric acid that the flow velocity of/h adds concentration, when system pH is 2.5, stops adding sulfuric acid, ageing 2h;
S3, the silica batch after ageing carried out press filtration washing, dry broken, obtain washing powder high specific surface area silica.
the preparation method of embodiment 2, washing powder high specific surface area silica of the present invention
S1, in retort, add 12m
3water, be heated to 70 DEG C, then add 144kg glycerine, stir;
S2, with 13m
3the flow velocity of/h adds the water glass 9.6m that concentration is 0.8mol/L
3, simultaneously with 2.4m
3it is 6mol/L sulfuric acid that the flow velocity of/h adds concentration, when system pH is 3.0, stops adding sulfuric acid, ageing 2h;
S3, the silica batch after ageing carried out press filtration washing, dry broken, obtain washing powder high specific surface area silica.
the preparation method of embodiment 3, washing powder high specific surface area silica of the present invention
S1, in retort, add 12m
3water, be heated to 70 DEG C, then add 192kg glycerine, stir;
S2, with 16m
3the flow velocity of/h adds the water glass 14.4m that concentration is 0.6mol/L
3, simultaneously with 2.8m
3it is 4mol/L sulfuric acid that the flow velocity of/h adds concentration, when system pH is 2.0, stops adding sulfuric acid, ageing 2h;
S3, the silica batch after ageing carried out press filtration washing, dry broken, obtain washing powder high specific surface area silica.
embodiment 4, washing powder containing washing powder high specific surface area silica of the present invention
Formula: washing powder high specific surface area silica 15%, sodium carbonate 20%, sodium sulfate 42.8%, Xylo-Mucine 1%, water 5%, aliphatic alcohol polyethenoxy (8) ether 6%, Witco 1298 Soft Acid 10%, essence 0.1% and white dyes 0.1% that embodiment 1 is obtained.
Preparation method: first washing powder high specific surface area silica, sodium carbonate, sodium sulfate and Xylo-Mucine are mixed, stir, add water, aliphatic alcohol polyethenoxy (8) ether and Witco 1298 Soft Acid again, stir, finally add essence and white dyes, granulation, screening, obtain washing powder.
comparative example one,
S1, in retort, add 12m
3water, be heated to 70 DEG C, then add 252kg glycerine, stir;
S2, with 15m
3the flow velocity of/h adds the water glass 12m that concentration is 0.7mol/L
3, simultaneously with 2.6m
3it is 5mol/L sulfuric acid that the flow velocity of/h adds concentration, when system pH is 2.5, stops adding sulfuric acid, ageing 2h;
S3, the silica batch after ageing carried out press filtration washing, dry broken, be precipitated silicon-dioxide.
comparative example two,
S1, in retort, add 12m
3water, be heated to 70 DEG C, then add 216kg glycerine, stir;
S2, with 15m
3the flow velocity of/h adds the water glass 12m that concentration is 0.7mol/L
3, simultaneously with 2.6m
3it is 5mol/L sulfuric acid that the flow velocity of/h adds concentration, when system pH is 4.0, stops adding sulfuric acid, ageing 2h;
S3, the silica batch after ageing carried out press filtration washing, dry broken, be precipitated silicon-dioxide.
comparative example three,
Choose the technical scheme of the embodiment one in Chinese patent application CN102002120A.
test example one,
Use full-automatic N2 adsorption specific surface and pore volume Porosimetry (model 3H-2000PS4) to detect the silicon-dioxide that embodiment 1 ~ 3 and comparative example one ~ tri-obtain, result is as following table 1.
Table 1 each silicon-dioxide detected result table
From upper table 1, (1) specific surface area of the washing powder high specific surface area silica that the embodiment of the present invention 1 ~ 3 is obtained, pore volume and aperture are all obviously greater than comparative example three, illustrate that the preparation method of washing powder high specific surface area silica of the present invention is better than the preparation method of comparative example three, wherein maximum with the specific surface area of the obtained silicon-dioxide of embodiment 1, pore volume and aperture, performance is best, illustrates that the preparation method of embodiment 1 is best; (2) the weight ratio 0.021:1 of comparative example one glycerine and water, in this proportioning, the specific surface area of obtained silicon-dioxide, pore volume and aperture are all little than embodiment 1, illustrate that the consumption of glycerine of the present invention is and the weight ratio of water (0.012 ~ 0.018): 1, this consumption can be good at the growth structure controlling silicon-dioxide, reaches the object improving pore volume aperture, specific surface area; (3) silicon-dioxide ageing under the environment of pH value 4.0 that comparative example two is obtained, its specific surface area, pore volume and aperture are also all little than embodiment 1, illustrate that in 2.0 ~ 3.0 environment, silicon-dioxide is carried out ageing soaks and can expand pore volume aperture further.
test example two,
According to GB/T13174-2008 " dress material washes the mensuration of agent detersive power and anti-stain deposition capability again by liquid ", the detersive power of the washing powder of embodiment 4 is detected, its detersive power (with standard washing powder ratio) is 1.40, relative standard's powder deposition ash content ratio is 1.8, meets the national standard of GB/T13171.2-2009 washing powder (without phosphorous).
Above-described embodiment is illustrative principle of the present invention and effect thereof only, but not for limiting the present invention.Any person skilled in the art scholar all without prejudice under spirit of the present invention and category, can modify above-described embodiment or changes.Therefore, such as have in art usually know the knowledgeable do not depart from complete under disclosed spirit and technological thought all equivalence modify or change, must be contained by claim of the present invention.
Claims (7)
1. a preparation method for washing powder high specific surface area silica, is characterized in that, comprises the following steps:
S1, in retort, add water, be heated to 65 ~ 75 DEG C, then add glycerine, stir;
S2, add water glass and sulfuric acid simultaneously, stop when system pH is 2.0 ~ 3.0 adding sulfuric acid, ageing 1.5 ~ 2.5h;
S3, the silica batch after ageing carried out press filtration washing, dry broken, obtain washing powder high specific surface area silica.
2. the preparation method of washing powder high specific surface area silica as claimed in claim 1, it is characterized in that, the weight ratio of described glycerine and water is (0.012 ~ 0.018): 1.
3. the preparation method of washing powder high specific surface area silica as claimed in claim 2, it is characterized in that, the weight ratio of described glycerine and water is 0.018:1.
4. the preparation method of washing powder high specific surface area silica as claimed in claim 1, it is characterized in that, the concentration of described water glass is 0.6 ~ 0.8mol/L, and the volume ratio of itself and water is (0.8 ~ 1.2): 1, and the flow velocity added is 13 ~ 16m
3/ h.
5. the preparation method of washing powder high specific surface area silica as claimed in claim 1, it is characterized in that, the concentration of described sulfuric acid is 4 ~ 6mol/L, and the flow velocity added is 2.4 ~ 2.8m
3/ h.
6. the washing powder high specific surface area silica obtained by the preparation method of the arbitrary described washing powder high specific surface area silica of claim 1 ~ 5, it is characterized in that, the specific surface area of described washing powder high specific surface area silica is 600 ~ 700m
2/ g, pore volume is 2.8 ~ 3.0cm
3/ g, aperture is 16 ~ 20nm.
7. the purposes of washing powder high specific surface area silica in washing powder as claimed in claim 6.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105858668A (en) * | 2016-03-30 | 2016-08-17 | 广州市飞雪材料科技有限公司 | Preparation method of silicon dioxide with high oil absorption value and high water absorption capacity for washing powder |
| CN107324346A (en) * | 2017-07-27 | 2017-11-07 | 广州市飞雪材料科技有限公司 | A kind of preparation method of high-specific surface area high oil absorption value silica |
| CN107445171A (en) * | 2017-06-30 | 2017-12-08 | 广州市飞雪材料科技有限公司 | A kind of preparation method of low index of refraction high transparency type silica |
| CN108046273A (en) * | 2018-01-29 | 2018-05-18 | 广州市飞雪材料科技有限公司 | A kind of preparation method of high adsorption silica |
| WO2020168662A1 (en) * | 2019-02-22 | 2020-08-27 | 广州市飞雪材料科技有限公司 | Low-density colored silica particles having porous structure, and preparation thereof |
| CN112250074A (en) * | 2020-10-26 | 2021-01-22 | 广州市飞雪材料科技有限公司 | Preparation method and application of silicon dioxide with high oil absorption and high specific surface area |
| CN114235525A (en) * | 2021-12-10 | 2022-03-25 | 江西业力医疗器械有限公司 | Permanent slide specimen manufacturing method |
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| CN104528738A (en) * | 2014-12-23 | 2015-04-22 | 肇庆金三江硅材料有限公司 | Method for preparing low-wear silica particles for toothpaste |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105858668A (en) * | 2016-03-30 | 2016-08-17 | 广州市飞雪材料科技有限公司 | Preparation method of silicon dioxide with high oil absorption value and high water absorption capacity for washing powder |
| CN105858668B (en) * | 2016-03-30 | 2017-03-22 | 广州市飞雪材料科技有限公司 | Preparation method of silicon dioxide with high oil absorption value and high water absorption capacity for washing powder |
| CN107445171A (en) * | 2017-06-30 | 2017-12-08 | 广州市飞雪材料科技有限公司 | A kind of preparation method of low index of refraction high transparency type silica |
| CN107445171B (en) * | 2017-06-30 | 2018-05-29 | 广州市飞雪材料科技有限公司 | A kind of preparation method of low index of refraction high transparency type silica |
| CN107324346A (en) * | 2017-07-27 | 2017-11-07 | 广州市飞雪材料科技有限公司 | A kind of preparation method of high-specific surface area high oil absorption value silica |
| CN108046273A (en) * | 2018-01-29 | 2018-05-18 | 广州市飞雪材料科技有限公司 | A kind of preparation method of high adsorption silica |
| WO2020168662A1 (en) * | 2019-02-22 | 2020-08-27 | 广州市飞雪材料科技有限公司 | Low-density colored silica particles having porous structure, and preparation thereof |
| CN112250074A (en) * | 2020-10-26 | 2021-01-22 | 广州市飞雪材料科技有限公司 | Preparation method and application of silicon dioxide with high oil absorption and high specific surface area |
| CN112250074B (en) * | 2020-10-26 | 2021-05-07 | 广州市飞雪材料科技有限公司 | Preparation method and application of silicon dioxide with high oil absorption and high specific surface area |
| CN114235525A (en) * | 2021-12-10 | 2022-03-25 | 江西业力医疗器械有限公司 | Permanent slide specimen manufacturing method |
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Address after: 526238 Yingbin Road 23, hi tech Zone, Guangdong, Zhaoqing Patentee after: Jinsanjiang (Zhaoqing) silicon material Co., Ltd Address before: 526238 Yingbin Road 23, hi tech Zone, Guangdong, Zhaoqing Patentee before: Zhaoqing Jinsanjiang Silicon Material Co., Ltd. |