CN104326476A - Method for preparing high-quality diatomite based on supersonic wave effect by hydrochloric acid method - Google Patents
Method for preparing high-quality diatomite based on supersonic wave effect by hydrochloric acid method Download PDFInfo
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- CN104326476A CN104326476A CN201410547157.6A CN201410547157A CN104326476A CN 104326476 A CN104326476 A CN 104326476A CN 201410547157 A CN201410547157 A CN 201410547157A CN 104326476 A CN104326476 A CN 104326476A
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Abstract
The invention relates to a method for preparing high-quality diatomite based on supersonic wave effect by a hydrochloric acid method, which takes diatomite concentrate obtained by preliminary purification as a raw material, diatomite concentrate and HCl are heated for reaction under supersonic wave effect, filtration is carried out to filter SigmaxTCln lyotrope and hydrochloric acid, and steps of washing, drying and calcining are carried out to remove organic impurity, carbon and water in micropore of diatomite to obtain high purity diatomite. According to the provided method, perfect biological porous active structure characteristic of diatomite amorphous SiO2 can be kept, the processed diatomite has advantages of high activity, high whiteness and low iron, the whiteness can reach 88-96, the diatomite SiO2 content is greater than 98%, iron content is lower than 0.4%, specific surface is greater than 20m<2>/g, and quality and usage performance of the product can be greatly increased.
Description
Technical field
The present invention relates to mineral to purify, specifically diatomite is refined, and the hydrochloric acid method particularly related to based on ul-trasonic irradiation prepares the diatomaceous method of high-quality.
Background technology
Diatomite is the silicoide that unbodied biology becomes ore deposit.Main chemical compositions is non-crystalline silica, and impurity component mainly comprises the Al of colloidal type
2o
3, Fe
2o
3, MnO, CaO, MgO, K
2o, Na
2o, P
2o
5with organic and bone water.Usually in white, canescence, light gray, light yellow and Dark grey, light weight porous.Along with the exhaustion of resource, high-quality diatomite is fewer and feweri, and low-quality diatomite reaches the diatomaceous quality of high-quality through processing modified activation, is the popular domain of low-quality diatomite exploitation.
The pore volume of diatom original soil is generally 0.45 ~ 0.98cm
3/ g.Just because of diatom shell, there is micropore that is a large amount of, ordered arrangement, thus make diatomite have very large specific surface area, due to diatomaceous special gap structure, make it have very strong adsorptivity, its chemical stability is high, except being dissolved in hydrofluoric acid, be insoluble to any strong acid, be soluble in alkali.The features such as diatomite has that unit weight is little, fusing point is high in addition, heat insulation, sound absorption.
Increasingly reduce under native production technology enters the background of industrialization with diatom ore dressing essence at high-quality diatomite resource, for the high-efficiency comprehensive utilization of the low-grade diatomite resource of China, the Sustainable development of super-cell industry and meet related application industry and all have great importance to the ever-increasing demand of high-quality diatomite.In diatomite, the existence of detrimental impurity element (as iron, manganese etc.) constrains diatomaceous quality, quality and range of application, the comparatively feasible method at present low-quality diatomite being made refinement treatment has alkali calcining, normal pressure boils acid wash, but the iron level after process is still very high, alkaline process has corrosion destruction to structure of diatomite, and the boil process environments of acid elution method of normal pressure is harsh, also there is mechanical impact damage to structure.
Summary of the invention
The object of the invention is for existing technique Problems existing, in order to better middle-low grade diatomite be carried out refining, modification, upgrading and raising, providing a kind of hydrochloric acid method based on ul-trasonic irradiation to prepare the diatomaceous method of high-quality.
Hydrochloric acid method based on ul-trasonic irradiation of the present invention prepares the diatomaceous method of high-quality, comprises the following steps:
1) diatomite of preliminary purification is dispersed to granularity and reaches 10 ~ 100 μm, obtain diatomite powder;
2) by step 1) the diatomite powder that obtains and mass concentration be the mixed in hydrochloric acid of 18 ~ 36%,
3) by through step 2) mixture that obtains is placed in airtight acidproof voltage-resistant reactor, and under ul-trasonic irradiation, carry out reacting by heating, the reaction times is 5 ~ 24h, temperature of reaction 60 ~ 100 DEG C;
4) cool, reactant is taken out from reactor, filtering liquid, washing, drying;
5) by step 4) the dry thing that obtains calcines 0.5 ~ 4h, calcining temperature 450 ~ 800 DEG C in an oxidizing environment, to remove organism, charcoal and diatomaceous skeletal water, obtains finished product after cooling.
The present invention is in step 2), HCl consumption is 2 ~ 5 times of ∑ (x × n); Wherein ∑ (x × n) is other oxide compounds T except Si oxide compound
n xo
m ythe number x of middle metal ion T and the summation of valency n product.
Other oxide compounds in diatomite powder except Si oxide compound and HCl react as follows:
∑[T
n xO
m y+(x×n)HCl→xTCl
n+yH
2O]
In step 3), described ultrasonic wave comes from the ultrasonic generator of inside reactor, or reactor is placed in outside ultrasonic environment.
Described step 3) in the resistance to pressure pressure of reactor be greater than 3MPa.
Further, in step 3) in, the reaction times is 10 ~ 15h.
In step 4) in, washing comprises ultrasonic washing and/or hot wash, shows neutral until diatomite adds pure water pH.Hot water temperature is 60 ~ 100 DEG C.
In step 4) in, drying temperature is 120 ~ 300 DEG C, time of drying 1 ~ 5h.
Preferably, in step 5), described calcining temperature is 500 ~ 600 DEG C.
The diatomite concentrate that method suitable treatment of the present invention obtains through preliminary purification.Preliminary purification comprises cleans with NaOH dispersion, PRIMARY STIRRING, and settling sand removing, is separated with NaOH dispersion, elementary suspension, settlement separate, and secondary suspends and is separated, and secondary stirring is cleaned, suspend for three times the processes such as separation.
The present invention utilizes ultrasonic wave to clean diatomite surfaces externally and internally, attachment crucial detrimental impurity (iron, manganese etc.) material over celite is effectively separated, be conducive to HCl (other mineral acid effect deviation) in a heated condition to accelerate to react with detrimental impurity to form easy molten muriate,---water in washing---drying---calcining removing organic impurity, carbon and diatomaceous micropore, obtains high-purity diatomite to elimination ∑ xTCln lyotrope and hydrochloric acid etc. after filtration.Present invention improves over the method for prior art technique, under the severe condition without the need to increasing excessive cost, the diatomite after process retains amorphous Si O
2perfect biological stephanoporate structural performance, does not add other material (as whitening agent etc.), so can not introduce impurity, the diatomite whiteness after process can arrive 88 ~ 96, and iron level is lower than 0.4%, and specific surface is greater than 20m
2/ g, diatomite SiO
2content is greater than 98%, obtains quality and the product using chemically reactive greatly to improve.
Accompanying drawing explanation
Fig. 1 is that the high reactivity high whiteness high purity diatomite SEM of gained of the present invention schemes.
Embodiment
Be described principle of the present invention and feature below, example, only for explaining the present invention, is not intended to limit scope of the present invention.
Embodiment 1
1, first the diatomite of preliminary purification is dispersed to granularity 50 ~ 100 μm;
2, be then the mixed in hydrochloric acid of 36% by diatomite powder and mass concentration after pulverizing, other oxide compounds in diatomite powder except Si oxide compound except in ul-trasonic irradiation stripping and with HCl rapid reaction, formation:
∑(T
n xO
m y+(x×n)HCl→xTCl
n+yH
2O)
HCl consumption is 5 times of ∑ (x × n).
3, be then placed in airtight acidproof withstand voltage reactor, reactor put into ultrasonic oscillator and reacts, temperature of reaction 100 DEG C, the reaction times is 20h;
4, reaction terminates, and is taken out by reactant, filtering liquid after cooling from reactor, through 90 DEG C of hot washes until diatomite adds pure water pH show neutrality, then at 300 DEG C of dry 5h.
5, dry thing is calcined 1h in an oxidizing environment, calcining temperature 500 DEG C, require that oxidation fully, by organism, carbon, the removing of diatomaceous skeletal water in diatomite, obtain finished product after cooling and diatomite can be kept active
The product diatomite powder whiteness obtained is 88 ~ 93, and iron level is lower than 0.4%, and specific surface is greater than 20m
2/ g, diatomite SiO
2content is greater than 98%, does not change diatomite amorphous Si O
2biological stephanoporate structural performance.This product can be used for food filtrate, agriculture medicine, chemical fertilizer, microbe carrier etc.
Embodiment 2
1, first the diatomite of preliminary purification is dispersed to granularity 25 ~ 50 μm μm;
2, be then the mixed in hydrochloric acid of 25% by diatomite powder and mass concentration after pulverizing, other oxide compounds in diatomite powder except Si oxide compound except in ul-trasonic irradiation stripping and with HCl rapid reaction, formation:
∑(T
n xO
m y+(x×n)HCl→xTCl
n+yH
2O)
HCl consumption is 4 times of ∑ (x × n).
3, be then placed in airtight acidproof withstand voltage reactor, reactor put into ultrasonic oscillator and reacts, temperature of reaction 80 DEG C, the reaction times is 12h;
4, reaction terminates, and is taken out by reactant, filtering liquid after cooling from reactor, through 60 DEG C of hot washes until diatomite adds pure water pH show neutrality, then at 250 DEG C of dry 3h.
5, dry thing is calcined 1h in an oxidizing environment, calcining temperature 750 DEG C, require that oxidation fully, by organism, carbon, the removing of diatomaceous skeletal water in diatomite, obtain finished product after cooling and diatomite can be kept active
The product diatomite powder whiteness obtained is 88 ~ 95, and iron level is lower than 0.4%, and specific surface is greater than 20m
2/ g, diatomite SiO
2content is greater than 98%, does not change diatomite amorphous Si O
2biological stephanoporate structural performance.This product can be used for industrial flocculating aids, catalyzer and carrier, sorbent material, abrasive, coating, friction materials, thermal insulation material, soundproof material, insulating material, plastics and rubber and papermaking filler, also can be used as flatting agent, brightening agent, waste water conditioner, reodorant, battery separator material etc.
Embodiment 3
1, first the diatomite of preliminary purification is dispersed to granularity 10 ~ 25 μm;
2, be then the mixed in hydrochloric acid of 20% by diatomite powder and mass concentration after pulverizing, other oxide compounds in diatomite powder except Si oxide compound except in ul-trasonic irradiation stripping and with HCl rapid reaction, formation:
∑(T
n xO
m y+(x×n)HCl→xTCl
n+yH
2O)
HCl consumption is 2 times of ∑ (x × n).
3, be then placed in airtight acidproof withstand voltage reactor, reactor put into ultrasonic oscillator and reacts, temperature of reaction 60 DEG C, the reaction times is 6h;
4, reaction terminates, and is taken out by reactant, filtering liquid after cooling from reactor, through 60 DEG C of hot water and supersound washing until diatomite adds pure water pH shows neutral, then at 150 DEG C of dry 2h.
5, dry thing is calcined 1h in an oxidizing environment, calcining temperature 600 DEG C, require that oxidation fully, by organism, carbon, the removing of diatomaceous skeletal water in diatomite, obtain finished product after cooling and diatomite can be kept active
The product diatomite powder whiteness obtained is 88 ~ 96, and iron level is lower than 0.4%, and specific surface is greater than 20m
2/ g, diatomite SiO
2content is greater than 98%, does not change diatomite amorphous Si O
2biological stephanoporate structural performance.This product can be used for industrial edible oil flocculating aids, catalyzer and the aspect such as coating, friction materials, thermal insulation material, plastics and rubber and papermaking filler, medicine, toothpaste, abrasive material and chemical reagent in the food industry, use iron-free diatomaceous earth as filter aid, the leaching content of iron in beverage can be greatly reduced, the leaching content of iron in reduction beer, utilizes diatomaceous porousness and ventilation property to be used successfully to serial cosmetics filler and sorbent material obtains good effect.
The foregoing is only better embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (9)
1. the hydrochloric acid method based on ul-trasonic irradiation prepares the diatomaceous method of high-quality, comprises the following steps:
1) diatomite of preliminary purification is dispersed to granularity and reaches 10 ~ 100 μm, obtain diatomite powder;
2) by step 1) the diatomite powder that obtains and mass concentration be the mixed in hydrochloric acid of 18 ~ 36%,
3) by through step 2) mixture that obtains is placed in airtight acidproof voltage-resistant reactor, and under ul-trasonic irradiation, carry out reacting by heating, the reaction times is 5 ~ 24h, temperature of reaction 60 ~ 100 DEG C;
4) cool, reactant is taken out from reactor, filtering liquid, washing, drying;
5) by step 4) the dry thing that obtains calcines 0.5 ~ 4h, calcining temperature 450 ~ 800 DEG C in an oxidizing environment, to remove organism, charcoal and diatomaceous skeletal water, obtains finished product after cooling.
2. method according to claim 1, is characterized in that: in step 2), HCl consumption is 2 ~ 5 times of ∑ (x × n);
Wherein ∑ (x × n) is other oxide compounds T except Si oxide compound
n xo
m ythe number x of middle metal ion T and the summation of valency n product.
3. method according to claim 1, is characterized in that: in step 3), described ultrasonic wave comes from the ultrasonic generator of inside reactor, or reactor is placed in outside ultrasonic environment.
4. method according to claim 1, is characterized in that: described step 3) in the resistance to pressure pressure of reactor be greater than 3MPa.
5. method according to claim 1, is characterized in that: in step 3) in, the reaction times is 10 ~ 15h.
6. method according to claim 1, is characterized in that: in step 4) in, washing comprises ultrasonic washing and/or hot wash, shows neutral until diatomite adds pure water pH.
7. method according to claim 6, is characterized in that: described hot water temperature is 60 ~ 100 DEG C.
8. method according to claim 1, is characterized in that: in step 4) in, drying temperature is 120 ~ 300 DEG C, time of drying 1 ~ 5h.
9. method according to claim 1, is characterized in that: in step 5), described calcining temperature is 500 ~ 600 DEG C.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105040089A (en) * | 2015-07-14 | 2015-11-11 | 江西理工大学 | Process for preparing nanometer quartz porous whiskers by closed system acidproof and pressure-resistant heating reaction system |
| PL442544A1 (en) * | 2022-10-17 | 2024-04-22 | Politechnika Warszawska | Method of diatomaceous earth bleaching |
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| CN1322673A (en) * | 2001-06-26 | 2001-11-21 | 中国科学院长春应用化学研究所 | Diatomite purifying treatment method |
| CN1618734A (en) * | 2004-08-31 | 2005-05-25 | 胡小钟 | Purification method of kieselguhr filler |
| CN103086383A (en) * | 2013-01-21 | 2013-05-08 | 中国高岭土有限公司 | Preparation method of high-quality diatomaceous earth product |
| CN103282309A (en) * | 2010-10-12 | 2013-09-04 | 埃吉斯药物股份公开有限公司 | Method for preparation of an excipient suitable for pharmaceutical use |
| CN103864080A (en) * | 2014-03-07 | 2014-06-18 | 韦仲华 | Treatment method of low-iron diatomite with high activity and high brightness |
-
2014
- 2014-10-16 CN CN201410547157.6A patent/CN104326476A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1322673A (en) * | 2001-06-26 | 2001-11-21 | 中国科学院长春应用化学研究所 | Diatomite purifying treatment method |
| CN1618734A (en) * | 2004-08-31 | 2005-05-25 | 胡小钟 | Purification method of kieselguhr filler |
| CN103282309A (en) * | 2010-10-12 | 2013-09-04 | 埃吉斯药物股份公开有限公司 | Method for preparation of an excipient suitable for pharmaceutical use |
| CN103086383A (en) * | 2013-01-21 | 2013-05-08 | 中国高岭土有限公司 | Preparation method of high-quality diatomaceous earth product |
| CN103864080A (en) * | 2014-03-07 | 2014-06-18 | 韦仲华 | Treatment method of low-iron diatomite with high activity and high brightness |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105040089A (en) * | 2015-07-14 | 2015-11-11 | 江西理工大学 | Process for preparing nanometer quartz porous whiskers by closed system acidproof and pressure-resistant heating reaction system |
| PL442544A1 (en) * | 2022-10-17 | 2024-04-22 | Politechnika Warszawska | Method of diatomaceous earth bleaching |
| WO2024084294A1 (en) * | 2022-10-17 | 2024-04-25 | Politechnika Warszawska | Process for bleaching diatomaceous earth |
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Application publication date: 20150204 |
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