CN1463923A - Process for preparing magnesium carbonate whisker - Google Patents
Process for preparing magnesium carbonate whisker Download PDFInfo
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- CN1463923A CN1463923A CN 02121351 CN02121351A CN1463923A CN 1463923 A CN1463923 A CN 1463923A CN 02121351 CN02121351 CN 02121351 CN 02121351 A CN02121351 A CN 02121351A CN 1463923 A CN1463923 A CN 1463923A
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- magnesium
- bicarbonate solution
- magnesium carbonate
- magnesium bicarbonate
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Abstract
The present invention is the process of preparing magnesium carbonate crystal whisker from magnesium bicarbonate solution. Into magnesium bicarbonate solution, proper amount of additive is added, and through controlling the crystallization condition, magnesium carbonate crystal whisker in different sizes is prepared. Thus obtained magnesium carbonate crystal whisker has diameter of 0.1-5 microns and length of 10-2000 microns, may be used as reinforcing material for paint, plastic, rubber, etc. and may be used also as the intermediate product for preparing high-purity magnesia and other magnesium salt. The present invention opens new way for the comprehensive utilization of magnesium salt and has excellent application foreground.
Description
Technical Field
The invention relates to the technical field of preparation chemical industry, in particular to a method for preparing magnesium carbonate whiskers from a magnesium bicarbonate aqueous solution.
Background
The magnesium carbonate whisker is a single crystal of magnesium carbonate, and compared with common basic magnesium carbonate, the crystal of the magnesium carbonate whisker is completely developed, and the whisker is colorless and transparent. The crystal contains few defects, the crystal contains few impurities, and the strength of the crystal is high. Therefore, the magnesium carbonate whisker can be used for preparing high-purity magnesium oxide, magnesium hydroxide, basic magnesium carbonate, magnesium sulfate, magnesium chloride, magnesium nitrate and other magnesium salt products. Meanwhile, because of the good mechanical property of the magnesium carbonate whisker, the magnesium carbonate whisker can also be directly used for enhancing and improving the performance of plastics, rubber, paint, ink and the like, and can also be used as a filter material.
At present, most of basic magnesium carbonate products are commonly produced at home and abroad, and the Chinese patent application names are as follows: the preparation of magnesium salt whisker is described in (patent application No. 99113254.8) and there is no report on magnesium carbonate whisker. At present, basic magnesium carbonate which is generally produced at home and abroad is amorphous secondary agglomerated particles, has a large specific surface area and a large number of impurities adsorbed on the surface, and has poor mechanical properties due to the particles obtained by secondary agglomeration, so that when the basic magnesium carbonate is used as a filler of a composite material in rubber and plastics, the mechanical properties of a base material can be reduced to different degrees. The magnesium carbonate whisker related by the invention is a single crystal of magnesium carbonate, has complete crystal development, is colorless and transparent, contains less impurities, can be used as an intermediate for preparing high-purity basic magnesium carbonate, magnesium sulfate, magnesium chloride, magnesium nitrate and other magnesium salt products, is a single crystal of magnesium carbonate, has less crystal defects and has strength close to the ideal strength of the crystal, and can enhance the mechanical property of the material when being used as a filler of a composite material. Therefore, the invention has good application prospect.
Disclosure of Invention
The invention aims to solve the defects of overlarge specific surface area, low purity and poor mechanical property of secondary agglomerated particles of basic magnesium carbonate, and aims to prepare magnesium carbonate whiskers which contain few impurities and can be used as intermediates for preparing high-purity basic magnesium carbonate, magnesium oxide, magnesium chloride and magnesium hydroxide and used for enhancing and modifying plastics, rubber, coatings, printing ink and the like; thereby providing a compound of formula MgCO3·nH2O, n ═ one magnesium carbonate whisker in (1-5) and preparation method.
The purpose of the invention is realized as follows:
the magnesium carbonate whisker provided by the invention comprises the following components: having the formula: MgCO3·nH2O and n are one of (1-5), and the magnesium carbonate whisker has a diameter of 0.1-5 μm and a length of 20-2000 μm. The reaction can have different n values according to different reaction conditions, and the crystal whisker of magnesium carbonate is obtained by controlling the reaction conditions.
The preparation method of the magnesium carbonate whisker provided by the invention has the following reaction principle:
1. pretreatment of magnesium bicarbonate solution
Preparing a magnesium bicarbonate solution, then filtering and refining the magnesium bicarbonate solution by adopting a common process, and adjusting the concentration of the magnesium bicarbonate solution to be 1-100 g/L based on the mass of the magnesium bicarbonate;
2. adding additives
Adding an additive into the solution of magnesium bicarbonate prepared in the step 1 to dissolve the additive, wherein the concentration of the additive in the whole system is 0.01-100 g/L;
3. reaction crystallization
Slowly heating the magnesium bicarbonate solution prepared in the step 2 to 20-90 ℃, stirring at the speed of 40-400 rpm, and reacting for 0.1-100 hours, wherein the components and specifications of the crystal whiskers to be produced are determined by the reaction time and the reaction temperature;
4. filtering, washing and drying
And (3) filtering and washing the slurry obtained after the reaction in the step (3) by adopting a common method, and drying the slurry for 0.5 to 5 hours at the temperature of between 80 and 150 ℃.
The magnesium bicarbonate solution comprises various soluble magnesium salts and ammonium bicarbonate (or ammonium carbonate) which are obtained by reaction, and the soluble magnesium salts comprise magnesium chloride, magnesium sulfate, magnesium nitrate and the like. The magnesium bicarbonate solution also comprises an aqueous solution of magnesium bicarbonate obtained by carrying out carbonization reaction on ore pulp obtained by calcining and digesting dolomite or magnesite or other minerals containing magnesium hydroxide, magnesium oxide and magnesium carbonate or industrial waste residues and carbon dioxide and filtering.
The additive comprises: sodium phosphate, sodium dihydrogen phosphate, disodium hydrogen phosphate, ammonium dihydrogen phosphate, diammonium hydrogen phosphate, potassium dihydrogen phosphate, dipotassium hydrogen phosphate, sodium dodecyl benzene sulfonate and polyethylene glycol.
The invention has the advantages that:
1. the invention has simple process, the required equipment is common industrial equipment, the used raw materials are common industrial raw materials,
the production cost is low.
2. The magnesium carbonate crystal whisker prepared by the invention is a single crystal of magnesium carbonate, the crystal growth is complete, and the crystal whisker is colorless
Transparent, contains few defects, contains few impurities, has high strength and has
Has good application prospect.
Description of the drawings FIG. 1 is a biological microscopic magnification 1 (640X) of magnesium carbonate whisker prepared by the invention, FIG. 2 is a biological microscopic magnification 2 (640X) of magnesium carbonate whisker prepared by the invention
Detailed Description
Example 1
Calcining 1000g of magnesite at 800 ℃ for 2 hours, digesting the calcined magnesite with 20kg of tap water into magnesium hydroxide slurry, cooling the magnesium hydroxide slurry to 40 ℃, introducing carbon dioxide gas to carry out carbonization reaction, and filtering the slurry after the reaction is carried out for 4 hours to obtain a magnesium bicarbonate aqueous solution. And (2) putting 1000ml of the obtained magnesium bicarbonate aqueous solution into a beaker, adding 1g of additive sodium dihydrogen phosphate, stirring at the speed of 5rpm, heating the beaker to 65 ℃ after the additive is completely dissolved, increasing the stirring speed to 120rpm, reacting for 30 minutes, filtering the obtained slurry, and washing with deionized water for 5 times, wherein each time is 300 ml. And drying the filter cake obtained after washing and filtering at 110 ℃ for 2 hours to obtain the crystal whisker of magnesium carbonate.
The whisker of magnesium carbonate obtained in this example was: having the formula: MgCO3·3H2O, the diameter is 0.2 to 0.8 μm, and the length of the whisker is 20 to 200 μm.
Example 2
The preparation method of magnesium bicarbonate solution is the same as example 1, taking 1000ml of magnesium bicarbonate aqueous solution to a beaker, adding 2g of additive ammonium dihydrogen phosphate, stirring at the speed of 5rpm, and after the additive is completely dissolved, putting the beaker into the beakerAfter heating the cup to 50 ℃ and increasing the stirring speed to 120rpm, after 40 minutes of reaction, the resulting slurry was filtered and washed 5 times with 300ml each with deionized water. And drying the filter cake obtained after washing and filtering at 110 ℃ for 2 hours to obtain the crystal whisker of magnesium carbonate. The whisker of magnesium carbonate obtained in this example was: having the formula: MgCO3·5H2O, the diameter is 0.1 to 0.5 μm, and the length of the whisker is 20 to 100 μm.
Example 3
80g of chemically pure ammonium bicarbonate and 120g of magnesium sulfate heptahydrate are respectively hydrothermally hydrolyzed with 1000ml of water and then mixed to obtain a mixed solution of magnesium bicarbonate and ammonium sulfate. 1000ml of the magnesium bicarbonate aqueous solution is taken into a beaker, 1g of sodium dodecyl benzene sulfonate is added, the mixture is stirred at the speed of 5rpm, after the additive is completely dissolved, the beaker is heated to 70 ℃, the stirring speed is increased to 100rpm, the reaction is carried out for 20 minutes, the obtained slurry is filtered, and the mixture is washed by deionized water for 5 times, 300ml each time. And drying the filter cake obtained after washing and filtering at 110 ℃ for 2 hours to obtain the crystal whisker of magnesium carbonate. The whisker of magnesium carbonate obtained in this example was: having the formula: MgCO3·3H2O, the diameter is 0.5 to 1 μm, and the length of the whisker is 60 to 200 μm.
Example 4
80g of chemically pure ammonium bicarbonate and 100g of magnesium chloride hexahydrate are respectively hydrothermally hydrolyzed by 1000ml of water and then mixed to obtain a mixed solution of magnesium bicarbonate and ammonium chloride. 1000ml of the magnesium bicarbonate aqueous solution is taken into a beaker, 1g of monopotassium phosphate is added, the mixture is stirred at the speed of 5rpm, after the additive is completely dissolved, the beaker is heated to 40 ℃, the stirring speed is increased to 100rpm, after the reaction is carried out for 120 minutes, the obtained slurry is filtered, and the mixture is washed by deionized water for 5 times, 300ml each time. And drying the filter cake obtained after washing and filtering at 110 ℃ for 2 hours to obtain the crystal whisker of magnesium carbonate.
The whisker of magnesium carbonate obtained in this example was: having the formula: MgCO3·3H2O, the diameter is 0.8 to 2 μm, and the length of the whisker is 100 to 200 μm.
Claims (6)
1. Carbonic acidThe magnesium whisker is characterized in that: having the formula: MgCO3·nH2O, wherein n is 1-5; the diameter of the magnesium carbonate whisker is 0.1-5 μm, and the length is 20-2000 μm.
2. A process for the production of magnesium carbonate whiskers as recited in claim 1, wherein: the method comprises the following steps:
(1) pretreatment of magnesium bicarbonate solution
Preparing a magnesium bicarbonate solution, then filtering and refining the magnesium bicarbonate solution by adopting a common process, and adjusting the concentration of the magnesium bicarbonate solution to be 1-100 g/L based on the mass of the magnesium bicarbonate;
(2) adding additives
Adding the additive into the solution of magnesium bicarbonate prepared in the step 1 to dissolve the additive, wherein the concentration of the additive in the whole system is 0.01-100 g/L;
(3) reaction crystallization
Slowly heating the magnesium bicarbonate solution prepared in the step 2 to 20-90 ℃, stirring at the speed of 40-400 rpm, and reacting for 0.1-100 hours, wherein the components and specifications of the crystal whiskers to be produced are determined by the reaction time and the reaction temperature;
(4) and (3) filtering, washing and drying the slurry obtained after the reaction in the step (3) by adopting a common method, and drying the slurry for 0.5 to 5 hours at the temperature of between 80 and 150 ℃.
3. The method for preparing magnesium carbonate whiskers as recited in claim 2, wherein: the magnesium bicarbonate solution comprises magnesium bicarbonate solution obtained by reacting various soluble magnesium salts with ammonium bicarbonate or ammonium carbonate.
4. The method for preparing magnesium carbonate whiskers from a magnesium bicarbonate solution as recited in claim 3, wherein: the soluble magnesium salt comprises magnesium chloride, magnesium sulfate and magnesium nitrate.
5. The method for preparing magnesium carbonate whiskers from a magnesium bicarbonate solution as recited in claim 2, wherein: the magnesium bicarbonate solution also comprises an aqueous solution of magnesium bicarbonate obtained by the carbonization reaction of ore pulp obtained by calcining and digesting dolomite or magnesite or other minerals containing magnesium hydroxide, magnesium oxide and magnesium carbonate or industrial waste residues and carbon dioxide and filtering.
6. The method for preparing magnesium carbonate whiskers from a magnesium bicarbonate solution as recited in claim 2, wherein the additive comprises: sodium phosphate, sodium dihydrogen phosphate, disodium hydrogen phosphate, ammonium dihydrogen phosphate, diammonium hydrogen phosphate, potassium dihydrogen phosphate, dipotassium hydrogen phosphate, sodium dodecyl benzene sulfonate and polyethylene glycol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021213518A CN1186256C (en) | 2002-06-14 | 2002-06-14 | Process for preparing magnesium carbonate whisker |
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| Application Number | Priority Date | Filing Date | Title |
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| CNB021213518A CN1186256C (en) | 2002-06-14 | 2002-06-14 | Process for preparing magnesium carbonate whisker |
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| CN1463923A true CN1463923A (en) | 2003-12-31 |
| CN1186256C CN1186256C (en) | 2005-01-26 |
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| CNB021213518A Expired - Fee Related CN1186256C (en) | 2002-06-14 | 2002-06-14 | Process for preparing magnesium carbonate whisker |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101498041B (en) * | 2009-01-23 | 2011-09-21 | 东北大学 | Preparation of magnesia crystal whisker |
| CN102718235A (en) * | 2012-06-27 | 2012-10-10 | 辽宁工程技术大学 | Method for preparing magnesium carbonate trihydrate crystal whiskers by adopting basic magnesium carbonate tetrahydrate |
| 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 |
| CN103738985A (en) * | 2013-11-27 | 2014-04-23 | 长春工业大学 | Simple nanometer magnesium oxide preparation method |
| CN104828847A (en) * | 2015-06-02 | 2015-08-12 | 天津中海油服化学有限公司 | Method for preparing nesquehonite whiskers and nano flaky basic magnesium carbonate |
| CN105460961A (en) * | 2016-01-14 | 2016-04-06 | 宋丽英 | Method for utilizing magnesium hydrogen carbonate solution for preparing crystal-water-free magnesium carbonate |
| CN107021514A (en) * | 2017-05-25 | 2017-08-08 | 河北镁神科技有限公司 | A kind of high pure spherical magnesium carbonate raw powder's production technology used for cosmetic |
| WO2024109477A1 (en) * | 2022-11-21 | 2024-05-30 | 湖南大学 | Metal smelting waste residue-derived material, preparation method therefor and application thereof |
-
2002
- 2002-06-14 CN CNB021213518A patent/CN1186256C/en not_active Expired - Fee Related
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101498041B (en) * | 2009-01-23 | 2011-09-21 | 东北大学 | Preparation of magnesia crystal whisker |
| CN102718235A (en) * | 2012-06-27 | 2012-10-10 | 辽宁工程技术大学 | Method for preparing magnesium carbonate trihydrate crystal whiskers by adopting basic magnesium carbonate tetrahydrate |
| 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 |
| CN103738985A (en) * | 2013-11-27 | 2014-04-23 | 长春工业大学 | Simple nanometer magnesium oxide preparation method |
| CN104828847A (en) * | 2015-06-02 | 2015-08-12 | 天津中海油服化学有限公司 | Method for preparing nesquehonite whiskers and nano flaky basic magnesium carbonate |
| CN105460961A (en) * | 2016-01-14 | 2016-04-06 | 宋丽英 | Method for utilizing magnesium hydrogen carbonate solution for preparing crystal-water-free magnesium carbonate |
| CN107021514A (en) * | 2017-05-25 | 2017-08-08 | 河北镁神科技有限公司 | A kind of high pure spherical magnesium carbonate raw powder's production technology used for cosmetic |
| CN107021514B (en) * | 2017-05-25 | 2019-10-29 | 河北镁神科技股份有限公司 | A kind of high pure spherical magnesium carbonate raw powder's production technology used for cosmetic |
| WO2024109477A1 (en) * | 2022-11-21 | 2024-05-30 | 湖南大学 | Metal smelting waste residue-derived material, preparation method therefor and application thereof |
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| Publication number | Publication date |
|---|---|
| CN1186256C (en) | 2005-01-26 |
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Granted publication date: 20050126 Termination date: 20120614 |