CN102390841B - Preparation method of loose sericite powder - Google Patents
Preparation method of loose sericite powder Download PDFInfo
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- CN102390841B CN102390841B CN2011102124753A CN201110212475A CN102390841B CN 102390841 B CN102390841 B CN 102390841B CN 2011102124753 A CN2011102124753 A CN 2011102124753A CN 201110212475 A CN201110212475 A CN 201110212475A CN 102390841 B CN102390841 B CN 102390841B
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Abstract
The invention discloses a preparation method of loose sericite powder, relating to the preparation method of loose sericite powder and solving the problems that the sericite powder prepared by using the prior art is not loose, larger in thickness and not easy to disperse in water. The preparation method comprises the following steps of: 1, stirring strong oxidized acid, potassium nitrate and raw sericite ore, adding a strong oxidizing agent and stirring to a mixture A; 2, putting the mixture A in a water bath, stirring, adding distilled water and stirring, and adding hydrogen peroxide and stirring to obtain a mixture B; 3, filtering, washing and drying the mixture B; 4, putting the sericite treated in the step 3 to distilled water, ultrasonically oscillating to obtain a sericite solution, filtering the sericite solution, and centrifuging to obtain supernatant liquor; and 5, putting the supernatant liquor to a supercritical reaction kettle, introducing a gas, and discharging the gas after the reaction is ended to obtain the loose sericite powder. The sericite powder prepared by using the preparation method disclosed by the invention has the advantages of lower thickness, smaller granularity and easiness in dispersion in an aqueous solution.
Description
Technical field
The present invention relates to a kind of preparation method of sericite powder.
Background technology
Sericite is a kind of very important non-metallic minerals, China's sericite mineral products aboundresources, and reserves are large, distribution is wide, and a lot of provinces have large sericite mica ore to exist.Common sericite in powder is hydrophilic mineral filler, now has been widely used in the industrial sectors such as pottery, coating, rubber.It is broken that the at present preparation of sericite powder is mainly adopted, the methods such as ball milling or grinding.It is unloose that but these methods obtain the sericite powder, and thickness is larger, is difficult for disperseing in water.
In order to widen the Application Areas of sericite, improve the practical value of sericite, in the urgent need to a kind of loose, can be at the sericite powder of water camber dispersion.
Summary of the invention
The present invention is that will to solve the sericite powder of existing method preparation loose, and thickness is larger, and the problem that is difficult for disperseing in water provides a kind of preparation method of loose sericite powder.
The preparation method of a kind of loose sericite powder of the present invention, carry out according to the following steps:
One, acid with strong oxidizing property and saltpetre are mixed, add the sericite raw ore again, stir 10～20min, then add strong oxidizer, the control temperature is 0～20 ℃, continues to stir 6～10 hours, gets mixture A; Two, the mixture A that step 1 is obtained places 35～40 ℃ water bath with thermostatic control, stirs 2～4 hours, then adds distilled water, and the control temperature of reaction continues to stir 1 hour at 90～95 ℃, then adds hydrogen peroxide and stirs 30min, gets mixture B; Three, the mixture B that step 2 is obtained is with 200～300 purpose filtered through gauze, is 8%～10% hydrochloric acid soln washing 6～8 times with mass concentration again, then uses distilled water wash 2～3 times, and oven dry gets the sericite after the processing; Four, the sericite after the step 3 processing is placed distilled water, sonic oscillation 5～10 hours obtains sericite solution, with sericite solution with 300～400 purpose filtered through gauze, filtrate is separated by supercentrifuge, and centrifuge speed is 1000r/min, obtains supernatant liquid; Five, the supernatant liquid that step 4 is obtained places the supercritical reaction still, passes into gas, is that 50～100MPa, temperature of reaction are under 50～80 ℃ the condition at pressure, reacts 5～10 hours, emits gas after the end, namely obtains the sericite powder that loosens; Wherein the mass ratio of sericite raw ore, acid with strong oxidizing property, saltpetre and strong oxidizer is 1: 23～27: 0.3～0.7: 2～4 in the step 1; In the step 2 among distilled water, hydrogen peroxide and the mixture A mass ratio of sericite raw ore be 18～22: 1～3: 1.
The sericite resource is abundanter, and the sericite mica ore of China is distributed more widely, and raw material easily obtains, thereby cost of the present invention is lower; Method of the present invention is simple and easy to realize, is fit to suitability for industrialized production, and free from environmental pollution.The sericite powder of the inventive method preparation is loose, and thickness is less, and granularity is less, is easy to disperse in aqueous solution.
Description of drawings
Fig. 1 is that the sericite powder of embodiment one preparation amplifies 2000 times SEM photo; Fig. 2 is that the sericite raw ore amplifies 1000 times SEM photo.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: the preparation method of a kind of loose sericite powder of present embodiment, carry out according to the following steps: one, acid with strong oxidizing property and saltpetre are mixed, add again the sericite raw ore, stir 10～20min, then add strong oxidizer, the control temperature is 0～20 ℃, continues to stir 6～10 hours, gets mixture A; Two, the mixture A that step 1 is obtained places 35～40 ℃ water bath with thermostatic control, stirs 2～4 hours, then adds distilled water, and the control temperature of reaction continues to stir 1 hour at 90～95 ℃, then adds hydrogen peroxide and stirs 30min, gets mixture B; Three, the mixture B that step 2 is obtained is with 200～300 purpose filtered through gauze, is 8%～10% hydrochloric acid soln washing 6～8 times with mass concentration again, then uses distilled water wash 2～3 times, and oven dry gets the sericite after the processing; Four, the sericite after the step 3 processing is placed distilled water, sonic oscillation 5～10 hours obtains sericite solution, with sericite solution with 300～400 purpose filtered through gauze, filtrate is separated by supercentrifuge, and centrifuge speed is 1000r/min, obtains supernatant liquid; Five, the supernatant liquid that step 4 is obtained places the supercritical reaction still, passes into gas, is that 50～100MPa, temperature of reaction are under 50～80 ℃ the condition at pressure, reacts 5～10 hours, emits gas after the end, namely obtains the sericite powder that loosens; Wherein the mass ratio of sericite raw ore, acid with strong oxidizing property, saltpetre and strong oxidizer is 1: 23～27: 0.3～0.7: 2～4 in the step 1; In the step 2 among distilled water, hydrogen peroxide and the mixture A mass ratio of sericite raw ore be 18～22: 1～3: 1.
The sericite resource is abundanter, and the sericite mica ore of China is distributed more widely, and raw material easily obtains, thereby the cost of present embodiment is lower; The method of present embodiment is simple and easy to realize, is fit to suitability for industrialized production, and free from environmental pollution.The sericite powder of present embodiment preparation is loose, and thickness is less, and granularity is less, is easy to disperse in aqueous solution.
The sericite powder of present embodiment preparation amplify 2000 times the SEM photo as shown in Figure 1, the sericite raw ore amplify 1000 times the SEM photo as shown in Figure 2, as can be seen from the figure the thickness of the sericite powder of present embodiment preparation is less, disperses comparatively even.
Embodiment two: what present embodiment and embodiment one were different is: the described acid with strong oxidizing property of step 1 is the salpeter solution of mass concentration 98% or the sulphuric acid soln of mass concentration 98%.Other is identical with embodiment one.
Embodiment three: what present embodiment was different from embodiment one or two is: the described strong oxidizer of step 1 is potassium permanganate or perchloric acid.Other is identical with embodiment one or two.
Embodiment four: what present embodiment was different from one of embodiment one to three is: the mass ratio of sericite raw ore, acid with strong oxidizing property, saltpetre and strong oxidizer is 1: 25: 0.5 in the step 1: 3.Other is identical with one of embodiment one to three.
Embodiment five: what present embodiment was different from one of embodiment one to four is: the control temperature is 0 ℃ in the step 1.Other is identical with one of embodiment one to four.
Embodiment six: what present embodiment was different from one of embodiment one to four is: the control temperature is 20 ℃ in the step 1.Other is identical with one of embodiment one to four.
Embodiment seven: what present embodiment was different from one of embodiment one to four is: the control temperature is 5～15 ℃ in the step 1.Other is identical with one of embodiment one to four.
Embodiment eight: what present embodiment was different from one of embodiment one to four is: the control temperature is 10 ℃ in the step 1.Other is identical with one of embodiment one to four.
Embodiment nine: what present embodiment was different from one of embodiment one to eight is: stirred 6 hours for the second time in the step 1.Other is identical with one of embodiment one to eight.
Embodiment ten: what present embodiment was different from one of embodiment one to eight is: stirred 10 hours for the second time in the step 1.Other is identical with one of embodiment one to eight.
Embodiment 11: what present embodiment was different from one of embodiment one to eight is: stirred 8 hours for the second time in the step 1.Other is identical with one of embodiment one to eight.
Embodiment 12: what present embodiment was different from one of embodiment one to 11 is: in the step 2 among distilled water, hydrogen peroxide and the mixture A mass ratio of sericite raw ore be 20: 2: 1.Other is identical with one of embodiment one to 11.
Embodiment 13: what present embodiment was different from one of embodiment one to 12 is: the water bath with thermostatic control that in the step 2 mixture A is placed 38 ℃.Other is identical with one of embodiment one to 12.
Embodiment 14: what present embodiment was different from one of embodiment one to 13 is: the control temperature of reaction is at 90 ℃ in the step 2.Other is identical with one of embodiment one to 13.
Embodiment 15: what present embodiment was different from one of embodiment one to 13 is: the control temperature of reaction is at 95 ℃ in the step 2.Other is identical with one of embodiment one to 13.
Embodiment 16: what present embodiment was different from one of embodiment one to 13 is: the control temperature of reaction is at 93 ℃ in the step 2.Other is identical with one of embodiment one to 13.
Embodiment 17: what present embodiment was different from one of embodiment one to 16 is: in the step 3 with mixture B with 200 purpose filtered through gauze.Other is identical with one of embodiment one to 16.
Embodiment 18: what present embodiment was different from one of embodiment one to 16 is: in the step 3 with mixture B with 300 purpose filtered through gauze.Other is identical with one of embodiment one to 16.
Embodiment 19: what present embodiment was different from one of embodiment one to 16 is: in the step 3 with mixture B with 250 purpose filtered through gauze.Other is identical with one of embodiment one to 16.
Embodiment 20: what present embodiment was different from one of embodiment one to 19 is: be the washing of 10% hydrochloric acid soln with mass concentration in the step 3.Other is identical with one of embodiment one to 19.
Embodiment 21: what present embodiment was different from one of embodiment one to 20 is: sonic oscillation is 5 hours in the step 4.Other is identical with one of embodiment one to 20.
Embodiment 22: what present embodiment was different from one of embodiment one to 20 is: sonic oscillation is 10 hours in the step 4.Other is identical with one of embodiment one to 20.
Embodiment 23: what present embodiment was different from one of embodiment one to 20 is: sonic oscillation is 7 hours in the step 4.Other is identical with one of embodiment one to 20.
Embodiment 24: what present embodiment was different from one of embodiment one to 23 is: in the step 4 with sericite solution with 300 purpose filtered through gauze.Other is identical with one of embodiment one to 23.
Embodiment 25: what present embodiment was different from one of embodiment one to 23 is: in the step 4 with sericite solution with 400 purpose filtered through gauze.Other is identical with one of embodiment one to 23.
Embodiment 26: what present embodiment was different from one of embodiment one to 23 is: in the step 4 with sericite solution with 350 purpose filtered through gauze.Other is identical with one of embodiment one to 23.
Embodiment 27: what present embodiment was different from one of embodiment one to 26 is: the gas that passes in the step 5 is carbon dioxide or rare gas element.Other is identical with one of embodiment one to 26.
Embodiment 28: what present embodiment was different from one of embodiment one to 27 is: pressure is 50MPa in the step 5.Other is identical with one of embodiment one to 27.
Embodiment 29: what present embodiment was different from one of embodiment one to 27 is: pressure is 100MPa in the step 5.Other is identical with one of embodiment one to 27.
Embodiment 30: what present embodiment was different from one of embodiment one to 27 is: pressure is 60～90MPa in the step 5.Other is identical with one of embodiment one to 27.
Embodiment 31: what present embodiment was different from one of embodiment one to 27 is: pressure is 80MPa in the step 5.Other is identical with one of embodiment one to 27.
Embodiment 32: what present embodiment was different from one of embodiment one to 31 is: temperature of reaction is 50 ℃ in the step 5.Other is identical with one of embodiment one to 31.
Embodiment 33: what present embodiment was different from one of embodiment one to 31 is: temperature of reaction is 80 ℃ in the step 5.Other is identical with one of embodiment one to 31.
Embodiment 34: what present embodiment was different from one of embodiment one to 31 is: temperature of reaction is 60 ℃ in the step 5.Other is identical with one of embodiment one to 31.
Embodiment 35: what present embodiment was different from one of embodiment one to 34 is: reaction is 5 hours in the step 5.Other is identical with one of embodiment one to 34.
Embodiment 36: what present embodiment was different from one of embodiment one to 34 is: reaction is 10 hours in the step 5.Other is identical with one of embodiment one to 34.
Embodiment 37: what present embodiment was different from one of embodiment one to 34 is: reaction is 8 hours in the step 5.Other is identical with one of embodiment one to 34.
Embodiment 38: the preparation method of a kind of loose sericite powder of present embodiment, carry out according to the following steps: one, sulphuric acid soln and the 2.5g saltpetre with 115mL mass concentration 98% mixes, add again 5g sericite raw ore, stir 20min, then add 15g potassium permanganate, the control temperature is 0 ℃, continues to stir 8 hours, gets mixture A; Two, the mixture A that step 1 is obtained places 38 ℃ water bath with thermostatic control, stirs 3 hours, then adds 200mL distilled water, the control temperature of reaction is at 95 ℃, continue to stir 1 hour, the hydrogen peroxide that then adds 12mL mass concentration 30% stirs 30min, gets mixture B; Three, the mixture B that step 2 is obtained is with 200 purpose filtered through gauze, is 10% hydrochloric acid soln washing 6 times with mass concentration again, then uses distilled water wash 3 times, and oven dry gets the sericite after the processing; Four, the sericite after the step 3 processing is placed distilled water, sonic oscillation 10 hours obtains sericite solution, with sericite solution with 300 purpose filtered through gauze, filtrate is separated by supercentrifuge, and centrifuge speed is 1000r/min, obtains supernatant liquid; Five, the supernatant liquid that step 4 is obtained places the supercritical reaction still, passes into carbon dioxide, is that 60MPa, temperature of reaction are under 70 ℃ the condition at pressure, reacts 8 hours, emits gas after the end, namely obtains the sericite powder that loosens; Wherein the mass ratio of sericite raw ore, acid with strong oxidizing property, saltpetre and strong oxidizer is 1: 25: 0.5 in the step 1: 3; In the step 2 among distilled water, hydrogen peroxide and the mixture A mass ratio of sericite raw ore be 20: 2: 1.
The sericite powder of present embodiment preparation loosens, and thickness is less, and granularity is less, is easy to disperse in aqueous solution.
Embodiment 39: the preparation method of a kind of loose sericite powder of present embodiment, carry out according to the following steps: salpeter solution and the 2.5g saltpetre of 115mL mass concentration 98% are mixed, add again 5g sericite raw ore, stir 15min, then add 15g potassium permanganate, the control temperature is 10 ℃, continues to stir 10 hours, gets mixture A; Two, the mixture A that step 1 is obtained places 38 ℃ water bath with thermostatic control, stirs 2 hours, then adds distilled water, and the control temperature of reaction continues to stir 1 hour at 95 ℃, and the hydrogen peroxide that then adds 12mL mass concentration 30% stirs 30min, gets mixture B; Three, the mixture B that step 2 is obtained is with 200 purpose filtered through gauze, is 10% hydrochloric acid soln washing 7 times with the 1000mL mass concentration again, then uses the 200mL distilled water wash 2 times, and oven dry gets the sericite after the processing; Four, the sericite after the step 3 processing is placed distilled water, sonic oscillation 7 hours obtains sericite solution, and sericite solution with 400 purpose filtered through gauze, is separated filtrate by supercentrifuge, and centrifuge speed is 1000r/min, obtains supernatant liquid; Five, the supernatant liquid that step 4 is obtained places the supercritical reaction still, passes into carbon dioxide, is that 80MPa, temperature of reaction are under 60 ℃ the condition at pressure, reacts 7 hours, emits gas after the end, namely obtains the sericite powder that loosens; Wherein the mass ratio of sericite raw ore, acid with strong oxidizing property, saltpetre and strong oxidizer is 1: 25: 0.5 in the step 1: 3; In the step 2 among distilled water, hydrogen peroxide and the mixture A mass ratio of sericite raw ore be 20: 2: 1.
The sericite powder of present embodiment preparation loosens, and thickness is less, and granularity is less, is easy to disperse in aqueous solution.
Claims (8)
1. the preparation method of a loose sericite powder, the preparation method who it is characterized in that the sericite powder that loosens, carry out according to the following steps: one, acid with strong oxidizing property and saltpetre are mixed, add again the sericite raw ore, stir 10～20min, then add strong oxidizer, the control temperature is 0～20 ℃, continue to stir 6～10 hours, get mixture A; Two, the mixture A that step 1 is obtained places 35～40 ℃ water bath with thermostatic control, stirs 2～4 hours, then adds distilled water, and the control temperature of reaction continues to stir 1 hour at 90～95 ℃, then adds hydrogen peroxide and stirs 30min, gets mixture B; Three, the mixture B that step 2 is obtained is with 200～300 purpose filtered through gauze, is 8%～10% hydrochloric acid soln washing 6～8 times with mass concentration again, then uses distilled water wash 2～3 times, and oven dry gets the sericite after the processing; Four, the sericite after the step 3 processing is placed distilled water, sonic oscillation 5～10 hours obtains sericite solution, with sericite solution with 300～400 purpose filtered through gauze, filtrate is separated by supercentrifuge, and centrifuge speed is 1000r/min, obtains supernatant liquid; Five, the supernatant liquid that step 4 is obtained places the supercritical reaction still, passes into gas, is that 50～100MPa, temperature of reaction are under 50～80 ℃ the condition at pressure, reacts 5～10 hours, emits gas after the end, namely obtains the sericite powder that loosens; Wherein acid with strong oxidizing property is the salpeter solution of mass concentration 98% or the sulphuric acid soln of mass concentration 98% in the step 1, and strong oxidizer is potassium permanganate or perchloric acid; The mass ratio of sericite raw ore, acid with strong oxidizing property, saltpetre and strong oxidizer is 1: 23～27: 0.3～0.7: 2～4 in the step 1; In the step 2 among distilled water, hydrogen peroxide and the mixture A mass ratio of sericite raw ore be 18～22: 1～3: 1.
2. the preparation method of a kind of loose sericite powder according to claim 1, the mass ratio that it is characterized in that sericite raw ore, acid with strong oxidizing property, saltpetre and strong oxidizer in the step 1 is 1: 25: 0.5: 3.
3. the preparation method of a kind of loose sericite powder according to claim 2, the mass ratio that it is characterized in that sericite raw ore among distilled water in the step 2, hydrogen peroxide and the mixture A is 20: 2: 1.
4. the preparation method of a kind of loose sericite powder according to claim 3 is characterized in that in the step 3 mixture B with 200 purpose filtered through gauze.
5. the preparation method of a kind of loose sericite powder according to claim 4 is characterized in that in the step 4 sericite solution with 300 purpose filtered through gauze.
6. the preparation method of a kind of loose sericite powder according to claim 5 is characterized in that the gas that passes in the step 5 is carbon dioxide or rare gas element.
7. the preparation method of a kind of loose sericite powder according to claim 6 is characterized in that temperature of reaction is 60 ℃ in the step 5.
8. the preparation method of a kind of loose sericite powder according to claim 7 is characterized in that in the step 5 reaction 8 hours.
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| CN105733312A (en) * | 2016-02-02 | 2016-07-06 | 安徽恒昊科技有限公司 | Preparation method of sericite nano micro-sheets |
| CN105733313A (en) * | 2016-02-02 | 2016-07-06 | 安徽恒昊科技有限公司 | Cosmetic sericite having easy dispersibility |
| CN105733314A (en) * | 2016-02-02 | 2016-07-06 | 安徽恒昊科技有限公司 | Method for preparing industrial-grade sericite powder |
| CN107754758A (en) * | 2017-10-30 | 2018-03-06 | 浙江秋氏环保科技发展有限公司 | A kind of technique for the restoration of the ecosystem agent for preparing magnetic sericite |
| CN107814390A (en) * | 2017-11-01 | 2018-03-20 | 山东圣泉新材料股份有限公司 | A kind of grapheme material combined mica, preparation method and purposes |
| CN110590226B (en) * | 2019-10-17 | 2020-11-03 | 霍邱县明楼琉璃瓦有限公司 | Preparation method of cement mortar additive for novel block wall |
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| JP2007254188A (en) * | 2006-03-22 | 2007-10-04 | Meiki Shu | Method for producing acid-expandable mica |
| CN101823723B (en) * | 2009-12-11 | 2012-07-25 | 李钦俊 | Process method for preparing ultra-fine high-brightness sericite powder by pyrophyllite |
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