CN103880033A - Method for producing aluminum borate or magnesium borate through reaction extrusion technology - Google Patents
Method for producing aluminum borate or magnesium borate through reaction extrusion technology Download PDFInfo
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- CN103880033A CN103880033A CN201410092726.2A CN201410092726A CN103880033A CN 103880033 A CN103880033 A CN 103880033A CN 201410092726 A CN201410092726 A CN 201410092726A CN 103880033 A CN103880033 A CN 103880033A
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Abstract
The invention discloses a method for producing aluminum borate or magnesium borate through reaction extrusion technology. The method comprises the following steps: (1) evenly mixing soluble borate, soluble aluminum salt or soluble magnesium salt, and then reacting and extruding on a double-screw extruder; (2) curing the product obtained in the step (1) for 4-48h at 20-80DEG C; then washing, filtering and drying the product to obtain aluminum borate or magnesium borate. Due to high torque and high rotating speed of the double-screw extruder, reactants can fast react, so that the reaction time can be shortened, and the energy consumption can be reduced. Moreover, aluminum borate or magnesium borate particles with particle sizes of less than 10mu m can be prepared.
Description
Technical field
The invention belongs to aluminum borate and magnesium borate preparing technical field, be specifically related to a kind of method of producing aluminum borate or magnesium borate with reaction extrusion process.
Background technology
Aluminum borate is water insoluble, is dissolved in acid, is mainly used in glass and ceramic industry, can be used as flame retardant compositions and uses, and has the fire-retardant function that brightens.At present, the preparation of aluminum borate mainly adopts the method for fluxing and hydrothermal method.The method of fluxing is taking the boron oxide such as alumina source and boric acid, sodium tetraborate sources such as Tai-Ace S 150, aluminum nitrate and aluminum chloride and the fusing assistant such as potassium sulfate, salt of wormwood as raw material, in High Temperature Furnaces Heating Apparatus, be heated to 900～1200 DEG C, reaction 1～8h, then cooling discharging, material water cooks off fusing assistant, after filtration the dry aluminum borate white powder that obtains of washing; Hydrothermal method is to stir in heated in water solution with borates such as aluminum soluble salt and amine borate, sodium tetraborate such as Tai-Ace S 150, aluminum nitrate and aluminum chloride, the dry aluminum borate white powder that obtains of filtration washing.
Magnesium borate is slightly soluble in water, is dissolved in acid, is mainly used in pharmaceutical industry, sanitas, sterilant, also can be used as flame retardant compositions.At present, the production method of magnesium borate be mainly sodium tetraborate and magnesium chloride in reactor, under the condition of heated and stirred, react 3～5h, after filtration, washing, dry making.
The aluminum borate obtaining due to aforesaid method or the particle diameter ratio of magnesium borate particle are larger, in perborate tetrahydrate aluminium or magnesium borate crystallisation process, easily sneak into by-product impurities, affect product performance.Given this, be necessary present aluminum borate and magnesium borate production technique to improve.
Summary of the invention
For solving the shortcoming and defect part of prior art, the object of the present invention is to provide a kind of method of producing aluminum borate or magnesium borate with reaction extrusion process.
For achieving the above object, the present invention adopts following technical scheme:
A method of producing aluminum borate or magnesium borate with reaction extrusion process, comprises the following steps:
(1) by the one in aluminum soluble salt and solubility magnesium salts, mix with solubility borate, after mixing, on twin screw extruder, react and extrude;
(2) by the product of step (1) at 20～80 DEG C of slaking 4～48h, to impel crystal to grow; Then by product washing, filtration and dry, obtain described aluminum borate or magnesium borate.
Preferably, aluminum soluble salt and solubility borate are respectively 1 part and 1 part according to aluminum ion and the boratory chemical equivalent of solubility, and solubility magnesium salts and solubility borate are respectively 1 part and 1 part according to magnesium ion and the boratory chemical equivalent of solubility.
Preferably, the reaction of twin screw extruder described in step (1) extrusion temperature is 50～100 DEG C.
Preferred, described reaction extrusion temperature is 80 DEG C.
Preferably, solubility borate described in step (1) is sodium tetraborate, potassium tetraborate or tetraboric acid ammonium; Described aluminum soluble salt is Tai-Ace S 150, aluminum nitrate or aluminum chloride; Described solubility magnesium salts is magnesium sulfate or magnesium chloride.
Described slaking refers to 20～80 DEG C of sealings preserves 4～48h.
Preferably, described in step (2), curing temperature is 30～80 DEG C.
Preferred, described curing temperature is 50～60 DEG C.
Preferably, described in step (2), the curing time is 12～24h.
Preferred, the described curing time is 24h.
Compared with prior art, the present invention has the following advantages and beneficial effect:
(1) the present invention is due to high moment of torsion and the high rotating speed of twin screw extruder, makes the reactant can rapid reaction, shortened the reaction times, reduces energy consumption.
(2) the present invention can make aluminum borate or the magnesium borate particle that particle diameter is less than 10 microns.
(3) the inventive method production cost is low, productive rate is high.
Brief description of the drawings
The infrared spectrogram of Fig. 1 aluminum borate that to be embodiment 1 make with comparative example 1;
The infrared spectrogram of Fig. 2 aluminum borate that to be embodiment 2 make with comparative example 1;
The infrared spectrogram of Fig. 3 aluminum borate that to be embodiment 3 make with comparative example 1;
The infrared spectrogram of Fig. 4 magnesium borate that to be embodiment 4 make with comparative example 2;
The infrared spectrogram of Fig. 5 magnesium borate that to be embodiment 5 make with comparative example 2;
The infrared spectrogram of Fig. 6 magnesium borate that to be embodiment 6 make with comparative example 2.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are not limited to this.The BT-9300H laser fineness gage that sreen analysis data in embodiment and comparative example that the present invention is all are produced by Dandong Bai Te Instrument Ltd. is measured, and the Spectrum Two infrared spectrometer that infrared detection collection of illustrative plates is produced by perkin elmer instrument (Shanghai) Co., Ltd. is measured.
A method of producing aluminum borate with reaction extrusion process, comprises the following steps:
(1) on twin screw extruder, react and extrude after 3420g Tai-Ace S 150 and 4020g sodium tetraborate are mixed; After extruding, reaction obtains white mud shape product; Reaction extrusion temperature is 80 DEG C;
(2) by the product of step (1) at 50 DEG C of slaking 24h; Then by product washing, filtration and dry, obtain white aluminum borate powder.After testing, to obtain the productive rate of product be 98% to the present embodiment.The sreen analysis of the aluminum borate of gained is in table 1, and Fig. 1 is shown in by infrared detection collection of illustrative plates.
Comparative example 1
By a method for water react industrial production aluminum borate, comprise the following steps:
(1) 342g Tai-Ace S 150 and 402g sodium tetraborate are dissolved respectively, be made into dilute solution, then two kinds of solution are mixed and are heated to 100 DEG C, maintain 8h;
(2) reaction is filtered, washs and dry after feed liquid being cooled to room temperature after finishing, and obtains white aluminum borate powder.After testing, the product yield that this comparative example obtains is 80%.The sreen analysis of the aluminum borate of gained is in table 1, and Fig. 1 is shown in by infrared detection collection of illustrative plates.
The sreen analysis of the aluminum borate that table 1 embodiment 1 and comparative example 1 make
| ? | Meso-position radius | Volume mean diameter | Area average diameter | Length mean diameter | Specific |
| Embodiment | |||||
| 1 | 4.563μm | 6.093μm | 2.951μm | 0.965μm | 1037.5m^2/kg |
| Comparative example 1 | 16.182μm | 17.277μm | 12.722μm | 3.201μm | 174.6m^2/kg |
The infrared detection collection of illustrative plates of Fig. 1 aluminum borate that to be embodiment 1 make with comparative example 1.The infared spectrum of the aluminum borate that the aluminum borate that embodiment 1 makes as can see from Figure 1 and comparative example 1 make is basic identical, and main absorption peak can be well corresponding; The particle diameter of the aluminum borate making due to embodiment 1 is smaller, so the infrared absorption peak of the aluminum borate that embodiment 1 makes is eager to excel than comparative example 1.Can see the aluminum borate that the granular size of the aluminum borate that the embodiment of the present invention 1 makes makes much smaller than prior art from the data of table 1.
A method of producing aluminum borate with reaction extrusion process, comprises the following steps:
(1) on twin screw extruder, react and extrude after 2130g aluminum nitrate and 1740g tetraboric acid ammonium are mixed; After extruding, reaction obtains white mud shape product; Reaction extrusion temperature is 50 DEG C;
(2) by the product of step (1) at 20 DEG C of slaking 48h; Then by product washing, filtration and dry, obtain white aluminum borate powder.After testing, to obtain the productive rate of product be 97% to the present embodiment.The sreen analysis of the aluminum borate of gained is in table 2, and Fig. 3 is shown in by infrared detection collection of illustrative plates.
The sreen analysis of the aluminum borate that table 2 embodiment 2 and comparative example 1 make
| ? | Meso-position radius | Volume mean diameter | Area average diameter | Length mean diameter | Specific |
| Embodiment | |||||
| 2 | 4.212μm | 5.068μm | 2.635μm | 0.902μm | 1156.2m^2/kg |
| Comparative example 1 | 16.182μm | 17.277μm | 12.722μm | 3.201μm | 174.6m^2/kg |
The infrared detection collection of illustrative plates of Fig. 2 aluminum borate that to be embodiment 2 make with comparative example 1.The infared spectrum of the aluminum borate that the aluminum borate that embodiment 2 makes as can see from Figure 2 and comparative example 1 make is basic identical, and main absorption peak can be well corresponding; The particle diameter of the aluminum borate making due to embodiment 2 is smaller, so the infrared absorption peak of the aluminum borate that embodiment 2 makes is eager to excel than comparative example 1.Can see the aluminum borate that the granular size of the aluminum borate that the embodiment of the present invention 2 makes makes much smaller than prior art from the data of table 2.
Embodiment 3
A method of producing aluminum borate with reaction extrusion process, comprises the following steps:
(1) on twin screw extruder, react and extrude after 1330g aluminum chloride and 2330g potassium tetraborate are mixed; After extruding, reaction obtains white mud shape product; Reaction extrusion temperature is 100 DEG C;
(2) by the product of step (1) at 80 DEG C of slaking 4h; Then by product washing, filtration and dry, obtain white aluminum borate powder.After testing, to obtain the productive rate of product be 96% to the present embodiment.The sreen analysis of the aluminum borate of gained is in table 3, and Fig. 3 is shown in by infrared detection collection of illustrative plates.
The sreen analysis of the aluminum borate that table 3 embodiment 3 and comparative example 1 make
| ? | Meso-position radius | Volume mean diameter | Area average diameter | Length mean diameter | Specific surface area |
| Embodiment 3 | 4.133μm | 4.838μm | 2.423μm | 0.851μm | 1209.0m^2/kg |
| Comparative example 1 | 16.182μm | 17.277μm | 12.722μm | 3.201μm | 174.6m^2/kg |
The infrared detection collection of illustrative plates of Fig. 3 aluminum borate that to be embodiment 3 make with comparative example 1.The infared spectrum of the aluminum borate that the aluminum borate that embodiment 3 makes as can see from Figure 3 and comparative example 1 make is basic identical, and main absorption peak can be well corresponding; The particle diameter of the aluminum borate making due to embodiment 3 is smaller, so the infrared absorption peak of the aluminum borate that embodiment 3 makes is eager to excel than comparative example 1.Can see the aluminum borate that the granular size of the aluminum borate that the embodiment of the present invention 3 makes makes much smaller than prior art from the data of table 3.
Embodiment 4
A method of producing magnesium borate with reaction extrusion process, comprises the following steps:
(1) 950g magnesium chloride and 2010g sodium tetraborate react and extrude after mixing on twin screw extruder; After extruding, reaction obtains white mud shape product; Reaction extrusion temperature is 80 DEG C;
(2) by the product of step (1) at 50 DEG C of slaking 24h; Then by product washing, filtration and dry, obtain white magnesium borate powder.After testing, to obtain the productive rate of product be 98% to the present embodiment.The sreen analysis of the magnesium borate of gained is in table 4, and Fig. 4 is shown in by infrared detection collection of illustrative plates.
Comparative example 2
By a method for water react industrial production magnesium borate, comprise the following steps:
(1) 475g magnesium chloride and 1005g sodium tetraborate are dissolved respectively, be made into dilute solution, then two kinds of solution are mixed and are heated to 100 DEG C in reactor, maintain 5h;
(2) reaction is filtered, washs and dry after feed liquid being cooled to room temperature after finishing, and obtains white magnesium borate powder.After testing, the product yield that this comparative example obtains is 84%.The sreen analysis of the magnesium borate of gained is in table 4, and Fig. 4 is shown in by infrared detection collection of illustrative plates.
The sreen analysis of the magnesium borate that table 4 embodiment 4 and comparative example 2 make
| ? | Meso-position radius | Volume mean diameter | Area average diameter | Length mean diameter | Specific surface area |
| Embodiment 4 | 5.16μm | 7.02μm | 2.73μm | 0.841μm | 902.3m^2/kg |
| Comparative example 2 | 15.47μm | 17.28μm | 10.48μm | 4.860μm | 211.9m^2/kg |
The infrared detection collection of illustrative plates of Fig. 4 magnesium borate that to be embodiment 4 make with comparative example 2.The infared spectrum of the magnesium borate that the magnesium borate that embodiment 4 makes as can see from Figure 4 and comparative example 2 make is basic identical, and main absorption peak can be well corresponding; The particle diameter of the magnesium borate making due to embodiment 4 is smaller, so the infrared absorption peak of the magnesium borate that embodiment 4 makes is eager to excel than comparative example 2.Can see the magnesium borate that the granular size of the magnesium borate that the embodiment of the present invention 4 makes makes much smaller than prior art from the data of table 4.
Embodiment 5
A method of producing magnesium borate with reaction extrusion process, comprises the following steps:
(1) on twin screw extruder, react and extrude after 1520g magnesium sulfate and 1740g tetraboric acid ammonium are mixed; After extruding, reaction obtains white mud shape product; Reaction extrusion temperature is 50 DEG C;
(2) by the product of step (1) at 20 DEG C of slaking 48h; Then by product washing, filtration and dry, obtain white magnesium borate powder.After testing, to obtain the productive rate of product be 96% to the present embodiment.The sreen analysis of the magnesium borate of gained is in table 5, and Fig. 5 is shown in by infrared detection collection of illustrative plates.
The sreen analysis of the magnesium borate that table 5 embodiment 5 and comparative example 2 make
| ? | Meso-position radius | Volume mean diameter | Area average diameter | Length mean diameter | Specific surface area |
| Embodiment 5 | 4.93μm | 6.69μm | 2.35μm | 0.772μm | 987.8m^2/kg |
| Comparative example 2 | 15.47μm | 17.28μm | 10.48μm | 4.860μm | 211.9m^2/kg |
The infrared detection collection of illustrative plates of Fig. 5 magnesium borate that to be embodiment 5 make with comparative example 2.The infared spectrum of the magnesium borate that the magnesium borate that embodiment 5 makes as can see from Figure 5 and comparative example 2 make is basic identical, and main absorption peak can be well corresponding; The particle diameter of the magnesium borate making due to embodiment 5 is smaller, so the infrared absorption peak of the magnesium borate that embodiment 5 makes is eager to excel than comparative example 2.Can see the magnesium borate that the granular size of the magnesium borate that the embodiment of the present invention 5 makes makes much smaller than prior art from the data of table 5.
A method of producing magnesium borate with reaction extrusion process, comprises the following steps:
(1) on twin screw extruder, react and extrude after 950g magnesium chloride and 2330g potassium tetraborate are mixed; After extruding, reaction obtains white mud shape product; Reaction extrusion temperature is 100 DEG C;
(2) by the product of step (1) at 80 DEG C of slaking 4h; Then by product washing, filtration and dry, obtain white magnesium borate powder.After testing, to obtain the productive rate of product be 95% to the present embodiment.The sreen analysis of the magnesium borate of gained is in table 6, and Fig. 6 is shown in by infrared detection collection of illustrative plates.
The sreen analysis of the magnesium borate that table 6 embodiment 6 and comparative example 2 make
| ? | Meso-position radius | Volume mean diameter | Area average diameter | Length mean diameter | Specific |
| Embodiment | |||||
| 6 | 4.80μm | 6.26μm | 2.16μm | 0.716μm | 1058.2m^2/kg |
| Comparative example 2 | 15.47μm | 17.28μm | 10.48μm | 4.860μm | 211.9m^2/kg |
The infrared detection collection of illustrative plates of Fig. 6 magnesium borate that to be embodiment 6 make with comparative example 2.The infared spectrum of the magnesium borate that the magnesium borate that embodiment 6 makes as can see from Figure 6 and comparative example 2 make is basic identical, and main absorption peak can be well corresponding; The particle diameter of the magnesium borate making due to embodiment 6 is smaller, so the infrared absorption peak of the magnesium borate that embodiment 6 makes is eager to excel than comparative example 2.Can see the magnesium borate that the granular size of the magnesium borate that the embodiment of the present invention 6 makes makes much smaller than prior art from the data of table 6.
Above-described embodiment is preferably embodiment of the present invention; but embodiments of the present invention are not restricted to the described embodiments; other any do not deviate from change, the modification done under spirit of the present invention and principle, substitutes, combination, simplify; all should be equivalent substitute mode, within being included in protection scope of the present invention.
Claims (8)
1. a method of producing aluminum borate or magnesium borate with reaction extrusion process, is characterized in that, comprises the following steps:
(1) by the one in aluminum soluble salt and solubility magnesium salts, mix with solubility borate, after mixing, on twin screw extruder, react and extrude;
(2) by the product of step (1) at 20～80 DEG C of slaking 4～48h; Then by product washing, filtration and dry, obtain described aluminum borate or magnesium borate.
2. method according to claim 1, is characterized in that, the reaction of twin screw extruder described in step (1) extrusion temperature is 50～100 DEG C.
3. method according to claim 2, is characterized in that, described reaction extrusion temperature is 80 DEG C.
4. method according to claim 1, is characterized in that, solubility borate described in step (1) is sodium tetraborate, potassium tetraborate or tetraboric acid ammonium; Described aluminum soluble salt is Tai-Ace S 150, aluminum nitrate or aluminum chloride; Described solubility magnesium salts is magnesium sulfate or magnesium chloride.
5. method according to claim 1, is characterized in that, described in step (2), curing temperature is 30～80 DEG C.
6. method according to claim 5, is characterized in that, described curing temperature is 50～60 DEG C.
7. method according to claim 1, is characterized in that, the curing time described in step (2) is 12～24h.
8. method according to claim 7, is characterized in that, the described curing time is 24h.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107128943A (en) * | 2017-06-23 | 2017-09-05 | 齐鲁工业大学 | A kind of method of the synthetically prepared aluminium borate powder of utilization sol-gel processing |
| CN108203440A (en) * | 2016-12-19 | 2018-06-26 | 华东师范大学 | The continuous synthesis technology of solvent-free twin-screw extrusion of three potassium fluoborate of aryl |
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Cited By (3)
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| CN108203440A (en) * | 2016-12-19 | 2018-06-26 | 华东师范大学 | The continuous synthesis technology of solvent-free twin-screw extrusion of three potassium fluoborate of aryl |
| CN108203440B (en) * | 2016-12-19 | 2020-08-25 | 华东师范大学 | Solvent-free double-screw extrusion continuous synthesis process of potassium aryl trifluoroborate |
| CN107128943A (en) * | 2017-06-23 | 2017-09-05 | 齐鲁工业大学 | A kind of method of the synthetically prepared aluminium borate powder of utilization sol-gel processing |
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Application publication date: 20140625 |