CN101049947A - Method for preparing potassium fluoride in high activity - Google Patents
Method for preparing potassium fluoride in high activity Download PDFInfo
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- CN101049947A CN101049947A CN 200710065877 CN200710065877A CN101049947A CN 101049947 A CN101049947 A CN 101049947A CN 200710065877 CN200710065877 CN 200710065877 CN 200710065877 A CN200710065877 A CN 200710065877A CN 101049947 A CN101049947 A CN 101049947A
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- Prior art keywords
- potassium fluoride
- high activity
- preparation
- potassium
- activity according
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- 230000000694 effects Effects 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 18
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 title claims description 130
- 239000011698 potassium fluoride Substances 0.000 title claims description 54
- 235000003270 potassium fluoride Nutrition 0.000 title claims description 54
- 239000007864 aqueous solution Substances 0.000 claims abstract description 26
- 238000006243 chemical reaction Methods 0.000 claims abstract description 23
- 239000000243 solution Substances 0.000 claims abstract description 16
- 239000000047 product Substances 0.000 claims abstract description 12
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 10
- 230000007062 hydrolysis Effects 0.000 claims abstract description 9
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 9
- 239000006228 supernatant Substances 0.000 claims abstract description 9
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 238000002360 preparation method Methods 0.000 claims description 24
- 238000002425 crystallisation Methods 0.000 claims description 16
- 230000008025 crystallization Effects 0.000 claims description 16
- 238000000967 suction filtration Methods 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 5
- 238000004062 sedimentation Methods 0.000 claims description 4
- 150000004683 dihydrates Chemical class 0.000 claims description 3
- 239000003960 organic solvent Substances 0.000 claims description 3
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 2
- 239000002250 absorbent Substances 0.000 claims description 2
- 239000001110 calcium chloride Substances 0.000 claims description 2
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 2
- 239000000706 filtrate Substances 0.000 claims description 2
- 238000004108 freeze drying Methods 0.000 claims description 2
- 238000004064 recycling Methods 0.000 claims description 2
- 238000000352 supercritical drying Methods 0.000 claims description 2
- 238000001035 drying Methods 0.000 abstract description 7
- 239000012065 filter cake Substances 0.000 abstract description 6
- 239000013078 crystal Substances 0.000 abstract description 5
- 238000005265 energy consumption Methods 0.000 abstract description 5
- 239000000126 substance Substances 0.000 abstract description 3
- 239000000411 inducer Substances 0.000 abstract 1
- 230000001376 precipitating effect Effects 0.000 abstract 1
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 18
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 9
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 9
- 239000007789 gas Substances 0.000 description 7
- 238000005406 washing Methods 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- 229960000935 dehydrated alcohol Drugs 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 229960001866 silicon dioxide Drugs 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
This invention relates to a method for preparing a chemical product, i.e., high-activity KF. This invention adopts the traditional method for preparing KF, i.e., neutralization method or hydrolysis method, which comprises: (1) preparing KF aqueous solution by neutralization method or hydrolysis method; (2) controlling the ratio of the raw materials to control the end pH value of the reaction as well as the final concentration of the reaction solution; (3) precipitating the reaction solution, and taking the supernatant to obtain KF aqueous solution; (4) cooling KF aqueous solution, and adding inducer to obtain KF crystal; (5) vacuum-filtering the KF crystal, and drying the filter cake to obtain high-activity KF product. The method large reduces the energy consumption for preparing high-activity KF.
Description
Technical field
The present invention relates to a kind of chemical products preparation method, particularly the potassium fluoride in high activity preparation method.
Background technology
Potassium monofluoride is one of the most frequently used fluorizating agent, and we can say without Potassium monofluoride does not have flourish fluorine chemical.And Potassium monofluoride is as fluorizating agent reactive behavior in most important period, as fluorizating agent, particularly the production of fine chemistry industry with use, potassium fluoride in high activity has common anhydrous potassium fluoride incomparable advantage.
At present, the technology that potassium fluoride in high activity production is the most generally adopted is: adopt advanced drying, disintegrating process on the basis of traditional Potassium monofluoride production technique, particularly select suitable tensio-active agent for use, carry out spraying drying again, thereby make the high reactivity product.And can not prepare the potassium fluoride in high activity product by the method for direct crystallization.Because how the cost of equipment of spray drying technology and production energy consumption all than higher, find the potassium fluoride in high activity preparation method of low input less energy-consumption extremely urgent.
Summary of the invention
Purpose of the present invention is intended to overcome the defective of prior art, and a kind of low input, less energy-consumption, highly purified potassium fluoride in high activity preparation method are provided.
The preparation method of potassium fluoride in high activity of the present invention is that traditional Potassium monofluoride preparation technology---neutralisation or hydrolysis method may further comprise the steps in employing:
A. make potassium fluoride aqueous solution with neutralisation or hydrolysis method;
B. control the material ratio of reaction raw materials,, finish to reacting with the terminal point pH value of control reaction solution and the ultimate density of reaction solution;
C. with the reaction solution sedimentation, get supernatant liquid, be potassium fluoride aqueous solution;
D. with the cooling of Potassium monofluoride clear liquid, add inductor, get the Potassium monofluoride crystallization;
E. behind the crystallisate suction filtration, filtration cakes torrefaction is promptly got the potassium fluoride in high activity product.
The described potassium fluoride aqueous solution concentration of step b is 20%～60%.
The terminal point pH value of the described reaction solution of step b is 6-13.
The described inductor add-on of steps d should be 0.01%～5% of potassium fluoride aqueous solution total amount.
The described cooling temperature of steps d is-20 ℃～40 ℃.
The described inductor of steps d is the water-absorbent material.
Described inductor is Potassium monofluoride, dihydrate of potassium fluoride, calcium chloride.
The described crystallization of step e is washed with organic solvent when suction filtration.
The described filtration cakes torrefaction of step e can adopt a kind of in vacuum-drying, vacuum lyophilization or the supercritical drying.
In the present invention, gained filtrate can be returned mother liquid recycling.
The preparation method of Potassium monofluoride of the present invention is on traditional Potassium monofluoride preparation technology's basis, and making the concentration of obtained potassium fluoride aqueous solution by control material concentration and material ratio is 20%～60%, and the terminal point pH value is between 6 to 13.The sedimentation of gained potassium fluoride aqueous solution is filtered, after temperature with potassium fluoride aqueous solution transfers to-20 ℃～40 ℃ again, in it, add 0.01%～5% inductor, potassium fluoride aqueous solution is promptly finished crystallization in moment, organic solvent washing is used in crystallization when suction filtration, can shorten the time of drying of filter cake and the specific surface area of the potassium fluoride in high activity of gained is further improved, crystallization can be obtained the potassium fluoride in high activity product through after the suitable drying treatment.According to the kinetics of crystallization principle because the crystallization of Potassium monofluoride finishes in moment, so the time that crystal is not grown up guarantee, thereby can obtain Potassium monofluoride crystal than small particle size., the present invention not only greatly reduces the energy consumption and the facility investment expense of producing potassium fluoride in high activity after taking above-mentioned technology, also reduced the requirement to the raw material of preparation potassium fluoride in high activity.
Description of drawings
Fig. 1 is the process flow diagram of preparation method's of the present invention neutralisation.
Fig. 2 is the process flow diagram of preparation method's of the present invention hydrolysis method.
Embodiment
Below in conjunction with embodiment the present invention is described in further detail, but be not limited to embodiment.
Embodiment 1
1) 1000g potassium hydroxide is dissolved in the 800g water obtains potassium hydroxide solution, feed hydrogen fluoride gas in potassium hydroxide solution, the feeding speed of hydrogen fluoride gas is advisable at 40-70 ℃ to keep temperature of reaction;
2) when the pH value of reaction solution reaches 7.1, stop to feed hydrogen fluoride gas, neutralization reaction is finished;
3) the reaction solution sedimentation is left standstill 12 hours after, get supernatant liquid;
4) supernatant liquor is being cooled to 21 ℃, is adding 0.5g Potassium monofluoride inductor, potassium fluoride aqueous solution is promptly finished crystallization in moment;
5) suction filtration also with after the saturated potassium fluoride aqueous solution washing, is put into vacuum chamber with filter cake and was promptly got potassium fluoride in high activity in dry 4 hours.
Embodiment 2
Under the identical situation of other conditions and embodiment 1, when the step 5) suction filtration, wash with dehydrated alcohol.
Embodiment 3
Under the identical situation of other conditions and embodiment 1, after step 4) moment crystallization is finished, in crystalline potassium fluoride aqueous solution, add a certain amount of dehydrated alcohol and fully stir after suction filtration again.
Embodiment 4
1) 1000g potassium hydroxide is dissolved in the 1000g water obtains potassium hydroxide solution, add hydrogen fluoride gas in potassium hydroxide solution, the feeding speed of hydrogen fluoride gas is advisable at 40～70 ℃ to keep temperature of reaction;
2) when the pH value of reaction solution reaches 8.2, stop to feed hydrogen fluoride, neutralization reaction is finished;
3) the reaction solution quiescent settling after 10 hours, is got supernatant liquid;
4) supernatant liquid is cooled to 10 ℃, adds 0.3g Potassium monofluoride inductor in it, potassium fluoride aqueous solution is promptly finished crystallization in moment;
5) suction filtration also with after the saturated potassium fluoride aqueous solution washing, promptly gets potassium fluoride in high activity product at vacuum drying oven after dry 4 hours with filter cake.
Embodiment 5
Under the identical situation of other conditions and embodiment 4, when the step 5) suction filtration, wash with dehydrated alcohol.
Embodiment 6
1) 100g potassium hydroxide is dissolved in the 150g water obtains potassium hydroxide solution, add hydrogen fluoride gas in potassium hydroxide solution, the feeding speed of hydrogen fluoride gas is advisable at 40～70 ℃ to keep temperature of reaction;
2) PH of solution stopped to feed hydrogen fluoride at 12 o'clock, and neutralization reaction is finished;
3) the reaction solution quiescent settling was got supernatant liquid after 12 hours;
4) supernatant liquor is cooled to-5 ℃, adds 2g dihydrate of potassium fluoride inductor, potassium fluoride aqueous solution is promptly finished crystallization in moment;
5) suction filtration also with after the saturated potassium fluoride aqueous solution washing, promptly gets the potassium fluoride in high activity product with filter cake at the vacuum drying oven inner drying after 4 hours.
Embodiment 7
Under the identical situation of other conditions and embodiment 6, when the step 5) suction filtration, wash with dehydrated alcohol.
Embodiment 8
The Repone K 300g of preparation 23%, and to drip concentration in it be 10% silicofluoric acid 600g, after finishing after the reaction with gained crystal filtering and washing to pH value 〉=5 of washings, with filter cake again with 110g potassium hydroxide at 400g, fully hydrolysis obtains precipitation of silica and potassium fluoride aqueous solution in the water about 105 ℃ after the hydrolysis, and silicon-dioxide is removed in centrifugation, promptly obtain potassium fluoride aqueous solution, reaction equation is as follows:
H
2SiF
6+2KCl→K
2SiF
6+2HCl
K
2SiF
6+4KOH→6KF+SiO
2↓+2H
2O
After the gained potassium fluoride aqueous solution is cooled to 10 ℃, think to add the 1g Potassium monofluoride in it, potassium fluoride aqueous solution is promptly finished crystallization in moment, suction filtration and wash with dehydrated alcohol after crystallization was put into the vacuum drying oven inner drying 4 hours, promptly get the potassium fluoride in high activity product.
Each embodiment potassium fluoride in high activity product analysis the results are shown in following table:
Claims (10)
1, a kind of preparation method of potassium fluoride in high activity, the present invention adopt traditional Potassium monofluoride preparation technology---neutralisation or hydrolysis method, it is characterized in that may further comprise the steps:
A. make potassium fluoride aqueous solution with neutralisation or hydrolysis method;
B. control the material ratio of reaction raw materials,, finish to reacting with the terminal point pH value of control reaction solution and the ultimate density of reaction solution;
C. with the reaction solution sedimentation, get supernatant liquid, be potassium fluoride aqueous solution;
D. with the cooling of Potassium monofluoride clear liquid, add inductor, get the Potassium monofluoride crystallization;
E. behind the crystallisate suction filtration, filtration cakes torrefaction is promptly got the potassium fluoride in high activity product.
2, the preparation method of potassium fluoride in high activity according to claim 1 is characterized in that the described potassium fluoride aqueous solution concentration of step b is 20%～60%.
3, the preparation method of potassium fluoride in high activity according to claim 1, the terminal point pH value that it is characterized in that the described reaction solution of step b is 6-13.
4, the preparation method of potassium fluoride in high activity according to claim 1 is characterized in that the described inductor add-on of steps d should be 0.01%～5% of potassium fluoride aqueous solution total amount.
5, the preparation method of potassium fluoride in high activity according to claim 1 is characterized in that the described cooling temperature of steps d is-20 ℃～40 ℃.
6, the preparation method of potassium fluoride in high activity according to claim 1 is characterized in that the described inductor of steps d is the water-absorbent material.
7, the preparation method of potassium fluoride in high activity according to claim 6 is characterized in that described inductor is Potassium monofluoride, dihydrate of potassium fluoride, calcium chloride etc.
8, the preparation method of potassium fluoride in high activity according to claim 1 is characterized in that the described crystallization of step e washs with organic solvent when suction filtration.
9, the preparation method of potassium fluoride in high activity according to claim 1 is characterized in that the described filtration cakes torrefaction of step e can adopt a kind of in vacuum-drying, vacuum lyophilization or the supercritical drying.
10, the preparation method of potassium fluoride in high activity according to claim 1 is characterized in that gained filtrate can return mother liquid recycling.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200710065877 CN101049947A (en) | 2007-05-15 | 2007-05-15 | Method for preparing potassium fluoride in high activity |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200710065877 CN101049947A (en) | 2007-05-15 | 2007-05-15 | Method for preparing potassium fluoride in high activity |
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| Publication Number | Publication Date |
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| CN101049947A true CN101049947A (en) | 2007-10-10 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200710065877 Pending CN101049947A (en) | 2007-05-15 | 2007-05-15 | Method for preparing potassium fluoride in high activity |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107032371A (en) * | 2017-02-28 | 2017-08-11 | 河北科技大学 | A kind of method that potassium fluoride is prepared by raw material of fluorite |
| CN107381602A (en) * | 2017-07-11 | 2017-11-24 | 山东理工大学 | A kind of preparation method of the homogeneous potassium fluoride of high activity |
| CN116873952A (en) * | 2023-07-31 | 2023-10-13 | 云南云天化股份有限公司 | Method for preparing high-activity potassium fluoride and co-producing white carbon black by using p-fluoronitrobenzene byproduct potassium chloride |
-
2007
- 2007-05-15 CN CN 200710065877 patent/CN101049947A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107032371A (en) * | 2017-02-28 | 2017-08-11 | 河北科技大学 | A kind of method that potassium fluoride is prepared by raw material of fluorite |
| CN107381602A (en) * | 2017-07-11 | 2017-11-24 | 山东理工大学 | A kind of preparation method of the homogeneous potassium fluoride of high activity |
| CN116873952A (en) * | 2023-07-31 | 2023-10-13 | 云南云天化股份有限公司 | Method for preparing high-activity potassium fluoride and co-producing white carbon black by using p-fluoronitrobenzene byproduct potassium chloride |
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