CN102718235A - Method for preparing magnesium carbonate trihydrate crystal whiskers by adopting basic magnesium carbonate tetrahydrate - Google Patents
Method for preparing magnesium carbonate trihydrate crystal whiskers by adopting basic magnesium carbonate tetrahydrate Download PDFInfo
- Publication number
- CN102718235A CN102718235A CN2012102153657A CN201210215365A CN102718235A CN 102718235 A CN102718235 A CN 102718235A CN 2012102153657 A CN2012102153657 A CN 2012102153657A CN 201210215365 A CN201210215365 A CN 201210215365A CN 102718235 A CN102718235 A CN 102718235A
- Authority
- CN
- China
- Prior art keywords
- magnesium carbonate
- slurries
- slurry
- carbonate trihydrate
- whisker
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention belongs to the field of mineral processing and particularly relates to a method for preparing magnesium carbonate trihydrate crystal whiskers by adopting basic magnesium carbonate tetrahydrate. The method comprises the following steps of preparing the basic magnesium carbonate tetrahydrate and water into slurry; dropwise adding ammonium bicarbonate solution into the slurry; adding sodium hydrogen phosphate accounting for 1.0 to 2.0 percent of the total mass of the slurry into the slurry in which the ammonium bicarbonate solution is dropwise added, and adding ammonia water to regulate and controlling the pH (Potential of hydrogen) to be in the range of 9.0 to 9.5; continuously stirring to perform the reaction for 60 minutes, wherein the stirring strength is 120r/min.; filtering the reacted slurry to obtain a solid substance and filtrate; cleaning the solid substance by deionized water; and finally washing with absolute ethyl alcohol and drying for 4h at a temperature of 50 DEG C to obtain the magnesium carbonate trihydrate crystal whisker product. According to the technical scheme disclosed by the invention, the method has simple production process and equipment, high product yield and low cost, has no environmental pollution, is a green production process and is easy to implement the industrial production.
Description
Technical field
The invention belongs to the mineral manufacture field, be specifically related to the method that a kind of employing four hydration magnesium basic carbonates prepare the magnesium carbonate trihydrate whisker.
Background technology
The magnesiumcarbonate of widespread use is magnesium basic carbonate in industry at present, and its chemistry is to be generally x MgCO
3Y Mg (OH)
2ZH
2O, but because magnesium basic carbonate is unformed secondary agglomeration particle, have bigger specific surface area; The impurity of surface adsorption is more; And its mechanical property is relatively poor, is used among rubber, the plastics as the weighting material of matrix material, can reduce the mechanical property of body material to some extent.
The magnesium carbonate trihydrate whisker is the single crystal of magnesiumcarbonate, and its chemical formula is MgCO
33H
2O; Compare with common magnesium basic carbonate; Magnesium carbonate trihydrate whisker crystal is not only grown complete, the whisker water white transparency, and also the defective that crystal comprised is few; Crystal intensity is high, and the magnesium carbonate trihydrate whisker can be used to prepare highly purified Natural manganese dioxide, Marinco H, magnesium basic carbonate, sal epsom, magnesium nitrate and other magnesium salts product.And owing to have the good mechanical performance, the magnesium carbonate trihydrate whisker not only can directly be used for the enhancing and the modification of plastics, rubber, coating, printing ink etc., and can be used as filtering material.
The method for preparing at present the magnesium carbonate trihydrate whisker mainly is a chemical precipitation method; Utilize magnesium elements and carbonate or supercarbonate reaction in magnesium salts chemical reagent, magnesium-containing mineral (like magnesite, rhombspar etc.) or the salt lake bittern, prepare the magnesium carbonate trihydrate crystal whisker products.But in present preparation method,, cause synthetic magnesium carbonate trihydrate crystal whisker products productive rate very low, be unfavorable for large-scale industrial production because the magnesium ion content in the above-mentioned magnesium salts raw material is lower.
Summary of the invention
Problem to above-mentioned prior art existence; The present invention provides a kind of employing four hydration magnesium basic carbonates to prepare the method for magnesium carbonate trihydrate whisker; Not only can improve the productive rate of preparation magnesium carbonate trihydrate whisker; And can obtain high-quality magnesium carbonate trihydrate crystal whisker products, for the magnesium salts product becomes more meticulous, high purification production provides technical scheme.
The technical scheme of realization the object of the invention is carried out according to following steps:
(1) with four hydration magnesium basic carbonates and water by weight 1: (15 ~ 20) are mixed with slurries; Slurries are heated to 40 ~ 50 ℃, in slurries, drip ammonium bicarbonate soln 60min, to slurries pH=8.0-8.5; Continue in the dropping process to stir; Obtain the reactant slip, wherein stirring intensity is 120r/min, and bicarbonate of ammonia concentration is 0.8 ~ 1.2mol/L;
(2) in the slurries that drip ammonium bicarbonate soln, add the Sodium phosphate, dibasic that accounts for slurries total mass 1.0 ~ 2.0%, and add ammoniacal liquor regulation and control pH=9.0 ~ 9.5, continue stirring reaction 60min; Stirring intensity is 120r/min, with reacted slurry filtration, obtains solid matter and filtrating; Solid matter is used washed with de-ionized water; Use absolute ethanol washing at last, under 50 ℃, carry out the 4h oven dry, obtain the magnesium carbonate trihydrate crystal whisker products.
In the filtrating that step (2) obtains, feed CO
2Gas stops ventilation when filtrating pH=7.8-8.2, the evaporative crystallization of will filtrate then, acquisition NH
4HCO
3Product is with the NH that obtains
4HCO
3Product is as the reaction mass bicarbonate of ammonia in the step (1), the recycle of realization response material.
Compared with prior art, characteristics of the present invention and beneficial effect are:
The present invention is to be raw material with low value-added magnesium basic carbonate common and the most the most frequently used in the industry; Itself and bicarbonate of ammonia are reacted; PH through regulation and control solution prepares high-purity magnesium salts magnesium carbonate trihydrate crystal whisker products, and the chemical equation of generation is: 4MgCO
3Mg (OH)
24H
2O+2NH
4HCO
3=MgCO
33H
2O+ (NH
4)
2CO
3+ 3H
2O;
(NH
4)
2CO
3+?H
2O+?CO
2=?2NH
4HCO
3。
Technical scheme production technique of the present invention and equipment thereof are simple, and product yield is high, and is with low cost; Non-environmental-pollution is green production process, is easy to realize suitability for industrialized production; Not only improved the productive rate of magnesium carbonate trihydrate crystal whisker products; Improve meticulous magnesium salts quality of chemical products simultaneously, increased the productivity of derived product, promoted the value of development self.
Description of drawings
Fig. 1 is a process flow sheet of the present invention;
Fig. 2 is the SEM photo of the magnesium carbonate trihydrate whisker of the embodiment of the invention 1 preparation;
Fig. 3 is the SEM photo of the magnesium carbonate trihydrate whisker of the embodiment of the invention 2 preparations;
Fig. 4 is the SEM photo of the magnesium carbonate trihydrate whisker of the embodiment of the invention 3 preparations;
Fig. 5 is the XRD figure spectrum of the magnesium carbonate trihydrate whisker of the embodiment of the invention 3 preparations.
Embodiment
The employed chemical reagent of the embodiment of the invention is commercial analytical pure rank reagent, and wherein the mass concentration of ammoniacal liquor is 28%;
The instrument model that SEM scanning is adopted in the embodiment of the invention is day island proper Tianjin SEM-SS550, and the instrument model that the XRD figure spectrum adopts is the DX-2000 of Japan.
Embodiment 1
With reaction mass by four scale formula magnesiumcarbonate: the weight ratio of water=1:15 is mixed with slurry; The regulation and control temperature of reaction is 50 ℃, in slurries, drips ammonium bicarbonate soln 60min, to slurries pH=8.0; Obtain the reactant slip; Wherein bicarbonate of ammonia concentration is 0.8mol/L, continues in the reaction process to stir, and stirring intensity is 120r/min;
After the ammonium bicarbonate soln interpolation finishes, in the reactant slip, add the Sodium phosphate, dibasic that accounts for pulp quality 2.0%, and regulate and control pH=9.0 with ammoniacal liquor; Continue stirring reaction 60min, stirring intensity is 120r/min, with reacted slurry filtration; Obtain solid matter and filtrating, solid matter with washed with de-ionized water 3 times, is used absolute ethanol washing at last; Under 50 ℃, carry out the 4h oven dry, obtain the magnesium carbonate trihydrate crystal whisker products.
In filtrating, feed CO
2Gas stops ventilation when filtrating pH=8, then with reaction solution low temperature evaporate to dryness, obtains NH
4HCO
3Product is with the NH that obtains
4HCO
3Product carries out recycle as reaction mass bicarbonate of ammonia.
Through above technology, prepare high-purity magnesium carbonate trihydrate crystal whisker products, its SEM photo is as shown in Figure 2, and the magnesium carbonate trihydrate crystal whisker products mean length of present embodiment preparation reaches 78 μ m, and average aspect ratio reaches 15.
Embodiment 2
With reaction mass by four scale formula magnesiumcarbonate: the weight ratio of water=1:18 is mixed with slurry; The regulation and control temperature of reaction is 40 ℃, in slurries, drips ammonium bicarbonate soln 60min, to slurries pH=8.2; Form the reactant slip; Wherein bicarbonate of ammonia concentration is 0.9mol/L, continues in the reaction process to stir, and stirring intensity is 120r/min;
After ammonium bicarbonate soln dropwises, in the reactant slip, add the Sodium phosphate, dibasic of pulp quality 1.5%, and regulate and control pH=9.3 with ammoniacal liquor; Continue stirring reaction 60min, stirring intensity is 120r/min, with reacted slurry filtration; Obtain solid matter and filtrating, solid matter with washed with de-ionized water 5 times, is used absolute ethanol washing at last; Under 50 ℃, carry out the 4h oven dry, obtain the magnesium carbonate trihydrate crystal whisker products.
In filtrating, feed CO
2Gas stops ventilation when filtrating pH=7.8, then with reaction solution low temperature evaporate to dryness, obtains NH
4HCO
3Product is with the NH that obtains
4HCO
3Product carries out recycle as reaction mass bicarbonate of ammonia.
Through above technology, prepare high-purity magnesium carbonate trihydrate crystal whisker products, its SEM photo is as shown in Figure 3, and the magnesium carbonate trihydrate crystal whisker products mean length of present embodiment preparation reaches 85 μ m, and average aspect ratio reaches 16.
Embodiment 3
With reaction mass by four scale formula magnesiumcarbonate: the weight ratio of water=1:20 is mixed with slurry; The regulation and control temperature of reaction is 45 ℃, in slurries, drips ammonium bicarbonate soln 60min, to slurries pH=8.5; Obtain the reactant slip; Wherein bicarbonate of ammonia concentration is 1.2mol/L, continues in the reaction process to stir, and stirring intensity is 120r/min;
After ammonium bicarbonate soln dropwises, in the reactant slip, add the Sodium phosphate, dibasic that accounts for pulp quality 1.0%, and regulate and control pH=9.5 with ammoniacal liquor; Continue stirring reaction 60min, stirring intensity is 120r/min, and reaction slurry is filtered; Obtain solid matter and filtrating, solid matter with washed with de-ionized water 5 times, is used absolute ethanol washing at last; Under 50 ℃, carry out the 4h oven dry, obtain the magnesium carbonate trihydrate crystal whisker products.
In filtrating, feed CO
2Gas stops ventilation when filtrating pH=8.2, then with reaction solution low temperature evaporate to dryness, obtains NH
4HCO
3Product is with the NH that obtains
4HCO
3Product carries out recycle as reaction mass bicarbonate of ammonia.
Through above technology; Prepare high-purity magnesium carbonate trihydrate crystal whisker products, its SEM photo and XRD figure spectrum are respectively like Fig. 4 and shown in Figure 5, and as can be seen from the figure the magnesium carbonate trihydrate whisker purity of present embodiment preparation is higher; The mean length of product reaches 75 μ m, and average aspect ratio reaches 14.
Claims (2)
1. method that adopts four hydration magnesium basic carbonates to prepare the magnesium carbonate trihydrate whisker is characterized in that carrying out according to following steps: (1) with four hydration magnesium basic carbonates and water by weight 1: (15 ~ 20) are mixed with slurries, and slurries are heated to 40 ~ 50 ℃; In slurries, drip ammonium bicarbonate soln 60min; To slurries pH=8.0-8.5, continue in the dropping process to stir, obtain the reactant slip; Wherein stirring intensity is 120r/min, and the concentration of bicarbonate of ammonia concentration solution is 0.8 ~ 1.2mol/L;
(2) in the slurries that drip ammonium bicarbonate soln, add the Sodium phosphate, dibasic that accounts for slurries total mass 1.0 ~ 2.0%, and add ammoniacal liquor regulation and control pH=9.0 ~ 9.5, continue stirring reaction 60min; Stirring intensity is 120r/min, with reacted slurry filtration, obtains solid matter and filtrating; Solid matter is used washed with de-ionized water; Use absolute ethanol washing at last, under 50 ℃, carry out the 4h oven dry, obtain the magnesium carbonate trihydrate crystal whisker products.
2. a kind of employing four hydration magnesium basic carbonates according to claim 1 prepare the method for magnesium carbonate trihydrate whisker, it is characterized in that in the filtrating that step (2) obtains, feeding CO
2Gas stops ventilation when filtrating pH=7.8-8.2, the evaporative crystallization of will filtrate then, acquisition NH
4HCO
3Product is with the NH that obtains
4HCO
3Product is as the reaction mass bicarbonate of ammonia in the step (1).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012102153657A CN102718235A (en) | 2012-06-27 | 2012-06-27 | Method for preparing magnesium carbonate trihydrate crystal whiskers by adopting basic magnesium carbonate tetrahydrate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012102153657A CN102718235A (en) | 2012-06-27 | 2012-06-27 | Method for preparing magnesium carbonate trihydrate crystal whiskers by adopting basic magnesium carbonate tetrahydrate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102718235A true CN102718235A (en) | 2012-10-10 |
Family
ID=46944145
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2012102153657A Pending CN102718235A (en) | 2012-06-27 | 2012-06-27 | Method for preparing magnesium carbonate trihydrate crystal whiskers by adopting basic magnesium carbonate tetrahydrate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102718235A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102936750A (en) * | 2012-11-14 | 2013-02-20 | 辽宁工程技术大学 | Process for preparing trihydrate magnesium carbonate crystal whiskers through microwave method |
| CN104291366A (en) * | 2014-11-03 | 2015-01-21 | 苏州市泽镁新材料科技有限公司 | Preparation method for nanometer magnesium carbonate crystal |
| CN104355329A (en) * | 2014-11-03 | 2015-02-18 | 苏州市泽镁新材料科技有限公司 | Method for preparing nano magnesium carbonate crystal |
| CN105271322A (en) * | 2015-09-28 | 2016-01-27 | 辽宁工程技术大学 | Preparation method of fascicular magnesium carbonate trihydrate crystals |
| CN106219580A (en) * | 2016-07-25 | 2016-12-14 | 成都市新都化工股份有限公司 | A kind of method preparing basic magnesium carbonate |
| CN115369473A (en) * | 2022-09-27 | 2022-11-22 | 河北工业大学 | High-added-value closed-loop process for preparing magnesium carbonate trihydrate crystal whiskers |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0302514A2 (en) * | 1987-08-06 | 1989-02-08 | Ustav Pro Vyzkum Rud | Process for the preparation of anhydrous magnesium carbonate |
| CN1401573A (en) * | 2002-09-13 | 2003-03-12 | 清华大学 | Method for integrated production of magnesium sulfate, magnesium carbonate and magnesium hydroxide from magnesite |
| CN1463923A (en) * | 2002-06-14 | 2003-12-31 | 中国科学院过程工程研究所 | Process for preparing magnesium carbonate whisker |
-
2012
- 2012-06-27 CN CN2012102153657A patent/CN102718235A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0302514A2 (en) * | 1987-08-06 | 1989-02-08 | Ustav Pro Vyzkum Rud | Process for the preparation of anhydrous magnesium carbonate |
| CN1463923A (en) * | 2002-06-14 | 2003-12-31 | 中国科学院过程工程研究所 | Process for preparing magnesium carbonate whisker |
| CN1401573A (en) * | 2002-09-13 | 2003-03-12 | 清华大学 | Method for integrated production of magnesium sulfate, magnesium carbonate and magnesium hydroxide from magnesite |
Non-Patent Citations (1)
| Title |
|---|
| 闫平科 等: "高长径比三水碳酸镁晶须的合成研究", 《人工晶体学报》, vol. 41, no. 1, 29 February 2012 (2012-02-29), pages 158 - 164 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102936750A (en) * | 2012-11-14 | 2013-02-20 | 辽宁工程技术大学 | Process for preparing trihydrate magnesium carbonate crystal whiskers through microwave method |
| CN102936750B (en) * | 2012-11-14 | 2015-04-08 | 辽宁工程技术大学 | Process for preparing trihydrate magnesium carbonate crystal whiskers through microwave method |
| CN104291366A (en) * | 2014-11-03 | 2015-01-21 | 苏州市泽镁新材料科技有限公司 | Preparation method for nanometer magnesium carbonate crystal |
| CN104355329A (en) * | 2014-11-03 | 2015-02-18 | 苏州市泽镁新材料科技有限公司 | Method for preparing nano magnesium carbonate crystal |
| CN105271322A (en) * | 2015-09-28 | 2016-01-27 | 辽宁工程技术大学 | Preparation method of fascicular magnesium carbonate trihydrate crystals |
| CN106219580A (en) * | 2016-07-25 | 2016-12-14 | 成都市新都化工股份有限公司 | A kind of method preparing basic magnesium carbonate |
| CN115369473A (en) * | 2022-09-27 | 2022-11-22 | 河北工业大学 | High-added-value closed-loop process for preparing magnesium carbonate trihydrate crystal whiskers |
| CN115369473B (en) * | 2022-09-27 | 2024-02-02 | 河北工业大学 | High added value closed loop process for preparing magnesium carbonate trihydrate whiskers |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US9422167B2 (en) | Method for forming basic nickel carbonate | |
| CN102718235A (en) | Method for preparing magnesium carbonate trihydrate crystal whiskers by adopting basic magnesium carbonate tetrahydrate | |
| CN101259968A (en) | Method for preparing trihydrated magnesium carbonate from magnesium chloride-containing bittern by using ammonium carbonate | |
| CN102602974A (en) | Method for producing less-barium fine strontium salts from celestite | |
| CN101708835B (en) | Production method of high-purity zinc phosphate | |
| CN109336161B (en) | CeO2 nanotube preparation method, CeO2 nanotube and application | |
| CN104478699B (en) | Preparation method of high-purity superfine cobalt oxalate powder | |
| CN105129866A (en) | Method of producing iron oxide red through iron sulfate hydrothermal process | |
| CN106558695A (en) | A kind of nickel cobalt aluminum complex hydroxide, nickel cobalt aluminium composite oxide and preparation method thereof | |
| CN112707428A (en) | Combined preparation method of nano calcium carbonate and pseudo-boehmite or white carbon black | |
| CN109574056B (en) | Composite inducer for in-situ template-induced synthesis of nano calcium carbonate and application thereof | |
| CN102703982B (en) | Method for preparing magnesium carbonate trihydrate crystal whisker by utilizing serpentine | |
| KR101078602B1 (en) | Manufacturing method of calcite | |
| CN101935866A (en) | Method for preparing flaky calcite calcium carbonate crystal | |
| CN110562991A (en) | Production method of white carbon black for high-oil-absorption carrier | |
| CN109706526A (en) | It is a kind of to prepare Dihydrate gypsum whiskers, the method for hemihydrate calcium sulfate crystal whisker and product as made from it | |
| CN101659416B (en) | Method for preparing white carbon black co-product calcium chloride | |
| CN116199270B (en) | Treatment process for reducing wastewater in cobalt oxide production process | |
| CN110436512B (en) | Zinc hydroxychloride crystal and preparation method thereof | |
| CN114988383B (en) | Efficient preparation method of battery-grade ferric phosphate | |
| CN111847518A (en) | Efficient recycling method of silicomanganese slag | |
| CN101837999B (en) | Preparation method of Beta-type aluminum hydroxide | |
| CN103012217A (en) | Method for preparing high-purity aminoguanidine bicarbonate | |
| CN105197969B (en) | Preparation method of millimeter-grade radial nesquehonite crystal | |
| CN108101115A (en) | A kind of hydro-thermal method prepares the method without sulphur figure water hydroxyl sarmientite |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20121010 |