CN101279737A - Preparation for orthosilicic acid - Google Patents
Preparation for orthosilicic acid Download PDFInfo
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- CN101279737A CN101279737A CNA2008100616959A CN200810061695A CN101279737A CN 101279737 A CN101279737 A CN 101279737A CN A2008100616959 A CNA2008100616959 A CN A2008100616959A CN 200810061695 A CN200810061695 A CN 200810061695A CN 101279737 A CN101279737 A CN 101279737A
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- China
- Prior art keywords
- solution
- orthosilicic acid
- preparation
- choline chloride
- orthosilicic
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/141—Feedstock
Abstract
The invention relates to a method for preparing orthosilicic acid, the chemical formula of orthosilicic acid is H4SiO4. The method is characterized by the following steps: A, SiO2 and water are mixed according to the weight ratio of 10-20:100 and strongly stirred and NaOH or KOH solution is dropped until the pH value reaches 8-9 below the temperature of 15 DEG C; B, under strong stirring, the mixture is oil-bath heated until the temperature comes to 50-55 DEG C and reacts for 2-3 hours to obtain even solution; C, the solution is cooled to room temperature and under strong stirring, CO2 gas is fed into the even solution until the pH value is less than or equal to 4; D, choline chloride is added, wherein the weight ratio of choline chloride and the solution obtained from the step C is 20-45:100, then stirred for 10-20 minutes to obtain stable orthosilicic acid solution, wherein, the silicon content of the stable orthosilicic acid solution is 2-2.5 percent. The method of the invention has low cost to prepare orthosilicic acid, environmentally friendly preparation technique and no hazardous and noxious substances discharging during the preparation process; the orthosilicic acid solution obtained has the advantages of multifunction and long preservation time.
Description
Technical field
The present invention relates to a kind of preparation method of orthosilicic acid.
Background technology
Silicon is considered to have vital role for forming and keeping reticular tissue, and silicon also helps the mineralization of bone, so silicon is essential for the normal development of bone and reticular tissue.
The silicon that exists with the orthosilicic acid form is for Al
+ 3Ion has very high avidity, and helps Al
+ 3Ionic is eliminated.Therefore it can reduce the toxic action of aluminium to bone and brain.
These data promptings are in the biological growth phase, and it is very useful particularly in time replenishing silicon when pathological state.
The metabolic subject matter of silicon is that it is difficult to absorb, though silicon is a kind of profuse element, its natural existing way is water-fast inorganic salt or amorphous clays, and the silicon that this natural form exists is to be absorbed by biology.
The silicon that we exist in the food mainly is the form appearance with silico-aluminate or silicon-dioxide, and bioavailability is poor.
Basically confirmed that now bioactive silicon must be water miscible, and solubleness depends on the quantity of own OH group on the Siliciumatom.In blood and EV liquid, silicon exists with hydrated form on the physiology, i.e. orthosilicic acid form H
4SiO
4Exist, its pH value with organism has nothing to do, and almost completely is to exist with its free form, and research shows: have only monomeric or oligomeric orthosilicic acid can pass through intestines barrier (P.Creach, J.Adrian, Med.Et Nut.1990,16 (2), 73-90).
Monomeric orthosilicic acid is approximately 10 up to concentration in the solution
-4Mol/L is metastable; But, when concentration increases, H
4SiO
4Molecule is in conjunction with the oligopolymer and the polymkeric substance that form orthosilicic acid, forms water-soluble little or water-fast colloidal solution or silicon gel at last, and the bioavailability of its silicon weakens.
The method of existing production higher concentration orthosilicic acid is to adopt acid very strong hydrochloric acid and can mix by acid-hydrolyzed silicon compound, prepare orthosilicic acid by hydrochloric acid, and the strongly-acid that utilizes hydrochloric acid is kept the low polymerization degree of orthosilicic acid, increase the stability of orthosilicic acid, this preparation method's shortcoming is that hydrochloric acid is a kind of volatile acid, and the gas HCl that volatilizes is a kind of toxic gas, is unfavorable for environmental protection.
Shortcomings such as the method for existing preparation orthosilicic acid is generally all made stablizer with glycerine, and this method exists orthosilicic acid solution preservation period not long, easily produces oil consumption, and is aging easily.
The invention provides a kind of economy, environmental protection, the orthosilicic acid preparation method of toxicological harmless material discharging.
Summary of the invention
The technical problem to be solved in the present invention is: the preparation method that a kind of orthosilicic acid is provided, it is low that this preparation method has a preparation cost, preparation technology's environmental protection can not discharged hazardous and noxious substances in the preparation process, and the orthosilicic acid solution of preparation has long advantage of shelf time.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of preparation method of orthosilicic acid, the chemical formula of this orthosilicic acid is H
4SiO
4, it is characterized in that adopting the following step:
A) with SiO
2With water by weight 10-20: 100 mix, and violent stirring below 15 ℃, drips NaOH or KOH solution, to pH value be 8-9;
B) under violent stirring, oil bath is heated to 50-55 ℃, reacts 2-3 hour to obtaining uniform solution;
C) be cooled to room temperature, under the violent stirring situation, in above-mentioned homogeneous solution, feed CO
2Gas is to PH≤4;
D) and then adding and step C) the gained solution weight is than being 20-45: 100 choline chloride 60, stirred 10-20 minute, and promptly obtain stable orthosilicic acid solution, the silicone content of this orthosilicic acid solution is 2%-2.5%.
Weight ratio of mixture as preferred version of the present invention: SiO2 and water is 15-20: 100; Control feeds CO
2The flow of gas is 0.01-0.05L/min; The weight and the step C of the choline chloride 60 that adds step D)) weight ratio of gained solution is 25-35: 100.
The present invention adopts cheap SiO
2Prepare the silicate Na of solubility with NaOH
2SiO
3, then to the silicate Na of solubility
2SiO
3Feed cheap CO in the solution
2Gas, preparation orthosilicic acid H
4SiO
4, greatly reduce orthosilicic acid H like this
4SiO
4Preparation cost, and present method preparation technology is simple.The present invention has overcome the technological deficiency that traditional technology need be used hydrochloric acid, and hydrochloric acid is volatile strong acid, and the gas HCl that volatilizes is toxic and harmful, and the present invention adopts nontoxic CO
2Gas prepares orthosilicic acid H
4SiO
4, than more environmental protection of traditional technology.
Orthosilicic acid H
4SiO
4Preparation process in add stablizer choline chloride 60 C
5H
14NClO, choline chloride 60 are one of VITAMIN, and the major ingredient of Yelkin TTS is very important to the growing of livestock and poultry, nutrition.Choline chloride 60 can prevent the accumulation of fat in the liver kidney, prevents lesion tissue, can strengthen physique and the resistance against diseases of livestock and poultry, improves the growth of animals or poultry rate, laying rate; Choline chloride 60 promotes fish growth and breeding in addition, improves the effect of survival rate; Choline chloride 60 also has certain effect to the normal function that guarantees animal nervous system.
The present invention adopts choline chloride 60 to make stablizer, and it is not long to have overcome the orthosilicic acid solution preservation period of using glycerine to do the stablizer existence in the traditional technology, easily produces oil consumption and easy aged defective.The present invention utilizes orthosilicic acid H
4SiO
4With choline chloride 60 C
5H
14NClO forms the method for complex compound, prepares the orthosilicic acid solution of siliceous 2%-2.5%, makes the orthosilicic acid H for preparing
4SiO
4More stable, the shelf time is longer, can stablize with the orthosilicic acid solution of the present invention's preparation and preserve 2-3.Present method combines orthosilicic acid and choline chloride 60 simultaneously, makes the orthosilicic acid solution for preparing with present method have multifunctionality.
In sum, it is low that beneficial effect of the present invention not only is to prepare the orthosilicic acid cost, and preparation technology's environmental protection can not discharged hazardous and noxious substances in the preparation process, and the orthosilicic acid solution of preparation has advantage multi-functional and that the shelf time is long.
Embodiment
Embodiment 1:
The preparation method of orthosilicic acid, carry out according to the following steps:
A) take by weighing the SiO of 200g
2Mix with the water of 2kg, carry out violent stirring with the rotating speed that per minute 800 changes,, drip 3N NaOH solution below 15 ℃ with agitator, to pH value be 8;
B) under violent stirring, oil bath is heated to 50 ℃, reacts 3 hours to obtaining uniform solution;
C) above-mentioned solution is carried out press filtration, remove the impurity in the solution;
D) solution is cooled to room temperature, under the violent stirring situation, in above-mentioned solution, feeds CO
2Gas, control feeds CO
2The flow of gas is 0.01L/min, is to stop to feed CO at 4 o'clock to PH
2
E) and then to step D) add choline chloride 60 in the gained solution, the weight of the choline chloride 60 that adds and the weight ratio of described solution are 20: 100, stirred 10 minutes with the rotating speed that per minute 400 changes with agitator, be the stable orthosilicic acid solution of siliceous 2%-2.5%.
Embodiment 2:
The preparation method of orthosilicic acid, carry out according to the following steps:
A) take by weighing the SiO of 300g
2Mix with the water of 2kg, carry out violent stirring with the rotating speed that per minute 800 changes,, drip 3N KOH solution below 15 ℃ with agitator, to pH value be 8.5;
B) under violent stirring, oil bath is heated to 53 ℃, reacts 2 hours to obtaining uniform solution;
C) above-mentioned solution is carried out press filtration, remove the impurity in the solution;
D) solution is cooled to room temperature, under the violent stirring situation, in above-mentioned solution, feeds CO
2Gas, control feeds CO
2The flow of gas is 0.03L/min, is to stop to feed CO at 3.5 o'clock to PH
2
E) and then to step D) add choline chloride 60 in the gained solution, the weight of the choline chloride 60 that adds and the weight ratio of described solution are 25: 100, stirred 10 minutes with the rotating speed that per minute 400 changes with agitator, be the stable orthosilicic acid solution of siliceous 2%-2.5%.
Embodiment 3:
The preparation method of orthosilicic acid, carry out according to the following steps:
A) take by weighing the SiO of 400g
2Mix with the water of 2kg, carry out violent stirring with the rotating speed that per minute 800 changes,, drip 3N NaOH solution below 15 ℃ with agitator, to pH value be 9;
B) under violent stirring, oil bath is heated to 55 ℃, reacts 2.5 hours to obtaining uniform solution;
C) above-mentioned solution is carried out press filtration, remove the impurity in the solution;
D) be cooled to room temperature, under the violent stirring situation, in above-mentioned solution, feed CO
2Gas, control feeds CO
2The flow of gas is 0.05L/min, is to stop to feed CO at 3 o'clock to PH
2
E) and then to step D) add choline chloride 60 in the gained solution, the weight of the choline chloride 60 that adds and the weight ratio of described solution are 45: 100, stirred 10 minutes with the rotating speed that per minute 400 changes with agitator, be the stable orthosilicic acid solution of siliceous 2%-2.5%.
Embodiment 4:
The preparation method of orthosilicic acid, carry out according to the following steps:
A) take by weighing the SiO of 300g
2Mix with the water of 2kg, carry out violent stirring with the rotating speed that per minute 800 changes,, drip 3N KOH solution below 15 ℃ with agitator, to pH value be 8.5;
B) under violent stirring, oil bath is heated to 55 ℃, reacts 2.5 hours to obtaining uniform solution;
C) above-mentioned solution is carried out press filtration, remove the impurity in the solution;
D) be cooled to room temperature, under the violent stirring situation, in above-mentioned solution, feed CO
2Gas, control feeds CO
2The flow of gas is 0.05L/min, is to stop to feed CO at 3 o'clock to PH
2
E) and then to step D) add choline chloride 60 in the gained solution, the weight of the choline chloride 60 that adds and the weight ratio of described solution are 35: 100, stirred 10 minutes with the rotating speed that per minute 400 changes with agitator, be the stable orthosilicic acid solution of siliceous 2%-2.5%.
Claims (4)
1, a kind of preparation method of orthosilicic acid, the chemical formula of this orthosilicic acid is H
4SiO
4, it is characterized in that adopting the following step:
A) with SiO
2With water by weight 10-20: 100 mix, and violent stirring below 15 ℃, drips NaOH or KOH solution, to pH value be 8-9;
B) under violent stirring, oil bath is heated to 50-55 ℃, reacts 2-3 hour to obtaining uniform solution;
C) solution is cooled to room temperature, under the violent stirring situation, in above-mentioned solution, feeds CO
2Gas is to PH≤4;
D) and then adding and step C) the gained solution weight is than being 20-45: 100 choline chloride 60, stirred 10-20 minute, and promptly obtain stable orthosilicic acid solution.
2, the preparation method of orthosilicic acid according to claim 1 is characterized in that: the weight ratio of mixture of SiO2 and water is 15-20: 100.
3, the preparation method of orthosilicic acid according to claim 1 is characterized in that: the flow that control feeds carbonic acid gas is 0.01-0.05L/min.
4, the preparation method of orthosilicic acid according to claim 1 is characterized in that: the weight and the step C of the choline chloride 60 that adds step D)) weight ratio of gained solution is 25-35: 100.
Priority Applications (1)
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CNA2008100616959A CN101279737A (en) | 2008-05-29 | 2008-05-29 | Preparation for orthosilicic acid |
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CNA2008100616959A CN101279737A (en) | 2008-05-29 | 2008-05-29 | Preparation for orthosilicic acid |
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2011009950A1 (en) | 2009-07-23 | 2011-01-27 | Societe Anonyme Des Eaux Minerales D'evian, "S.A.E.M.E" | A process for producing water enriched with natural orthosilicic acid |
CN106883824A (en) * | 2015-12-15 | 2017-06-23 | 中国科学院大连化学物理研究所 | The preparation method of heat-storage thermoregulation polyethylene glycol/silicon oxide compound composite phase-change material |
PL424606A1 (en) * | 2018-02-16 | 2019-08-26 | Centrum Badawczo-Rozwojowe Glokor Spółka Z Ograniczoną Odpowiedzialnością | Method for production of concentrate for production of silicon compounds containing health-oriented beverage, used as the enterotransporter or enterosorbent and the modular system for production of concentrate |
CN113271927A (en) * | 2018-11-09 | 2021-08-17 | 生物矿物股份有限公司 | Water-soluble silicon-containing particles |
WO2024078282A1 (en) * | 2022-10-10 | 2024-04-18 | 淄博乐悠悠农业科技有限公司 | Liquid dressing for promoting wound healing |
-
2008
- 2008-05-29 CN CNA2008100616959A patent/CN101279737A/en active Pending
Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2011009950A1 (en) | 2009-07-23 | 2011-01-27 | Societe Anonyme Des Eaux Minerales D'evian, "S.A.E.M.E" | A process for producing water enriched with natural orthosilicic acid |
CN102665447A (en) * | 2009-07-23 | 2012-09-12 | 埃维昂矿泉水有限公司 | A process for producing water enriched with natural orthosilicic acid |
CN102665447B (en) * | 2009-07-23 | 2014-03-19 | 埃维昂矿泉水有限公司 | A process for producing water enriched with natural orthosilicic acid |
CN106883824A (en) * | 2015-12-15 | 2017-06-23 | 中国科学院大连化学物理研究所 | The preparation method of heat-storage thermoregulation polyethylene glycol/silicon oxide compound composite phase-change material |
CN106883824B (en) * | 2015-12-15 | 2019-09-13 | 中国科学院大连化学物理研究所 | Heat-storage thermoregulation polyethylene glycol/silicon oxide compound composite phase-change material preparation method |
PL424606A1 (en) * | 2018-02-16 | 2019-08-26 | Centrum Badawczo-Rozwojowe Glokor Spółka Z Ograniczoną Odpowiedzialnością | Method for production of concentrate for production of silicon compounds containing health-oriented beverage, used as the enterotransporter or enterosorbent and the modular system for production of concentrate |
CN113271927A (en) * | 2018-11-09 | 2021-08-17 | 生物矿物股份有限公司 | Water-soluble silicon-containing particles |
WO2024078282A1 (en) * | 2022-10-10 | 2024-04-18 | 淄博乐悠悠农业科技有限公司 | Liquid dressing for promoting wound healing |
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Open date: 20081008 |