CN103879979A - Method for producing aluminium hypophosphite by adopting reaction extrusion process - Google Patents
Method for producing aluminium hypophosphite by adopting reaction extrusion process Download PDFInfo
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- CN103879979A CN103879979A CN201410093156.9A CN201410093156A CN103879979A CN 103879979 A CN103879979 A CN 103879979A CN 201410093156 A CN201410093156 A CN 201410093156A CN 103879979 A CN103879979 A CN 103879979A
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Abstract
The invention discloses a method for producing aluminium hypophosphite by adopting a reaction extrusion process. The method comprises the following steps: (1) uniformly mixing hypophosphite and aluminium salt or hypophosphorous acid and aluminium hydroxide or hypophosphorous acid and aluminium oxide, and carrying out reaction extrusion on a double screw extruder; (2) aging a product obtained from the step (1) at 20-80 DEG C for 4-48 hours, and then washing, filtering and drying the product to obtain the aluminium hypophosphite. According to the method, a reactant can be fast reacted due to high torque and high rotation speed of the double screw extruder, so that the reaction time can be shortened, and the energy consumption can be reduced; an aluminium hypophosphite granule with the grain diameter less than 10 micrometers can be obtained.
Description
Technical field
The invention belongs to hypo-aluminum orthophosphate preparing technical field, be specifically related to a kind of method of producing hypo-aluminum orthophosphate with reaction extrusion process.
Background technology
Hypo-aluminum orthophosphate is a kind of novel inorganic phosphorus flame retardant, chemical formula is Al (H2PO2) 3, there is the advantages such as the water of being slightly soluble in water, not volatile, phosphorus content is high, Heat stability is good, make its application product have that flame retardant resistance is high, thermostability strong and mechanical property and the excellent feature of weathering resistance.At present, it is raw material that the production of hypo-aluminum orthophosphate mainly adopts sodium hypophosphite and Tai-Ace S 150, and in water, reacting by heating obtains hypo-aluminum orthophosphate particle, after being dried, obtains dry powder through pulverizing.
The particle diameter of the hypo-aluminum orthophosphate particle obtaining due to aforesaid method is larger, easily sneaks into the crystallization of sodium sulfate byproduct in the process of hypo-aluminum orthophosphate crystallization, causes the decomposition temperature of the finished product hypo-aluminum orthophosphate obtaining to reduce.Given this, be necessary existing hypo-aluminum orthophosphate 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 hypo-aluminum orthophosphate with reaction extrusion process.
For achieving the above object, the present invention adopts following technical scheme:
A method of producing hypo-aluminum orthophosphate with reaction extrusion process, comprises the following steps:
(1) by hypophosphite and aluminium salt, or Hypophosporous Acid, 50 and aluminium hydroxide, or Hypophosporous Acid, 50 and aluminum oxide, after mixing, on twin screw extruder, react and extrude;
(2) by the product of step (1) at 20～80 ℃ of slaking 4～48h, to impel crystal to grow; Then product is washed successively, filtered and be dried, obtain described hypo-aluminum orthophosphate.
Preferably, hypophosphite and aluminium salt are respectively 3 parts and 1 part according to hypophosphite ion and aluminum ions chemical equivalent, and Hypophosporous Acid, 50 and aluminium hydroxide are respectively 5 parts and 2 parts according to mass ratio, and Hypophosporous Acid, 50 and aluminum oxide are respectively 19 parts and 5 parts according to mass ratio.
Preferably, to react the temperature of extruding be 40～80 ℃ to the described twin screw extruder of step (1).
Preferred, the temperature that described reaction is extruded is 50 ℃.
Preferably, the described hypophosphite of step (1) is sodium hypophosphite, potassium hypophosphite or ammonium hypophosphite; Described aluminium salt is Tai-Ace S 150, aluminum chloride or aluminum nitrate.
Described slaking refers to 20～80 ℃ of sealings preserves 4～48h.
Preferably, the described curing temperature of step (2) is 30～80 ℃.
Preferred, described curing temperature is 50～60 ℃.
Preferably, the described curing time of step (2) 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) due to high moment of torsion and the high rotating speed of twin screw extruder, reactant can rapid reaction, and therefore, energy Reaction time shorten of the present invention, reduces energy consumption.
(2) the present invention can obtain the hypo-aluminum orthophosphate particle that particle diameter is less than 10 microns.
(3) the inventive method production cost is low, productive rate is high.
Accompanying drawing explanation
The infrared spectrogram of Fig. 1 hypo-aluminum orthophosphate that to be embodiment 1 make with comparative example 1;
The hot weightless picture of Fig. 2 hypo-aluminum orthophosphate that to be embodiment 1 make with comparative example 1;
The infrared spectrogram of Fig. 3 hypo-aluminum orthophosphate that to be embodiment 2 make with comparative example 1;
The hot weightless picture of Fig. 4 hypo-aluminum orthophosphate that to be embodiment 2 make with comparative example 1;
The infrared spectrogram of Fig. 5 hypo-aluminum orthophosphate that to be embodiment 3 make with comparative example 1;
The hot weightless picture of Fig. 6 hypo-aluminum orthophosphate that to be embodiment 3 make with comparative example 1;
The infrared spectrogram of Fig. 7 hypo-aluminum orthophosphate that to be embodiment 4 make with comparative example 1;
The hot weightless picture of Fig. 8 hypo-aluminum orthophosphate that to be embodiment 4 make with comparative example 1;
The infrared spectrogram of Fig. 9 hypo-aluminum orthophosphate that to be embodiment 5 make with comparative example 1;
The hot weightless picture of Figure 10 hypo-aluminum orthophosphate that to be embodiment 5 make with comparative example 1.
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, the Spectrum Two infrared spectrometer that infrared detection collection of illustrative plates is produced by perkin elmer instrument (Shanghai) Co., Ltd. is measured, and the TGA4000 thermogravimetric analyzer that hot weightless picture and decomposition temperature are produced by perkin elmer instrument (Shanghai) Co., Ltd. is measured.
Embodiment 1
A method of producing hypo-aluminum orthophosphate with reaction extrusion process, comprises the following steps:
(1) 5280g sodium hypophosphite and 3420g Tai-Ace S 150 are mixed, then compound being added to Temperature Setting is to react and extrude in the twin screw extruder of 50 ℃; Extrude and obtain white mud shape product through reaction;
(2) product of step (1) is preserved to slaking 24h at the environment lower seal of 50 ℃; Then by product washing, filtration and dry, obtain the hypo-aluminum orthophosphate of white powder.After testing, to obtain the productive rate of product be 98% to the present embodiment.The sreen analysis of the hypo-aluminum orthophosphate of gained is in table 1, and Fig. 1 is shown in by infrared detection collection of illustrative plates, and hot weightless picture is shown in Fig. 2 and table 2.
Comparative example 1
By a method for water react explained hereafter hypo-aluminum orthophosphate, comprise the following steps:
(1) 528g sodium hypophosphite and 342g Tai-Ace S 150 are dissolved into respectively to dilute solution, then two kinds of solution are mixed and are heated to 100 ℃, maintain 12h;
(2) reaction finish after by feed liquid filtered while hot, washing, dries, and obtains the hypo-aluminum orthophosphate of white powder.After testing, to obtain the productive rate of product be 85% to this comparative example.The sreen analysis of the hypo-aluminum orthophosphate of gained is in table 1, and Fig. 1 is shown in by infrared detection collection of illustrative plates, and hot weightless picture is shown in Fig. 2 and table 2.
The sreen analysis of the hypo-aluminum orthophosphate that table 1 embodiment 1 and comparative example 1 make
| ? | Meso-position radius | Volume mean diameter | Area average diameter | Length mean diameter | Specific surface area |
| Embodiment 1 | 3.164μm | 5.585μm | 1.159μm | 0.313μm | 1916m^2/kg |
| Comparative example 1 | 24.61μm | 32.27μm | 10.31μm | 1.926μm | 215.3m^2/kg |
The decomposition temperature analysis of the hypo-aluminum orthophosphate that table 2 embodiment 1 and comparative example 1 make
Can see the hypo-aluminum orthophosphate that the granular size of the hypo-aluminum orthophosphate that the embodiment of the present invention 1 makes makes much smaller than prior art from table 1.The infrared detection collection of illustrative plates of Fig. 1 hypo-aluminum orthophosphate that to be embodiment 1 make with comparative example 1.The infared spectrum of the hypo-aluminum orthophosphate that the hypo-aluminum orthophosphate that embodiment 1 makes as can see from Figure 1 and comparative example 1 make is basic identical, and main absorption peak can be on deserved; The particle diameter of the hypo-aluminum orthophosphate making due to embodiment 1 is smaller, so the infrared absorption peak of the hypo-aluminum orthophosphate that embodiment 1 makes is eager to excel than comparative example 1.The hot weightless picture of Fig. 2 hypo-aluminum orthophosphate that to be embodiment 1 make with comparative example 1.The decomposition temperature that can see the hypo-aluminum orthophosphate that the embodiment of the present invention 1 makes from Fig. 2 and table 2 is greater than the hypo-aluminum orthophosphate that prior art makes.
Embodiment 2
A method of producing hypo-aluminum orthophosphate with reaction extrusion process, comprises the following steps:
(1) 2490g ammonium hypophosphite and 2130g aluminum nitrate are mixed, then compound being added to Temperature Setting is to react and extrude in the twin screw extruder of 70 ℃; Extrude and obtain white mud shape product through reaction;
(2) product of step (1) is preserved to slaking 4h at the environment lower seal of 80 ℃; Then by product washing, filtration and dry, obtain the hypo-aluminum orthophosphate of white powder.After testing, to obtain the productive rate of product be 97% to the present embodiment.The sreen analysis of the hypo-aluminum orthophosphate of gained is in table 3, and Fig. 3 is shown in by infrared detection collection of illustrative plates, and hot weightless picture is shown in Fig. 4 and table 4.
The sreen analysis of the hypo-aluminum orthophosphate that table 3 embodiment 2 and comparative example 1 make
| ? | Meso-position radius | Volume mean diameter | Area average diameter | Length mean diameter | Specific surface area |
| Embodiment 2 | 3.846μm | 6.258μm | 1.648μm | 0.431μm | 1032m^2/kg |
| Comparative example 1 | 24.61μm | 32.27μm | 10.31μm | 1.926μm | 215.3m^2/kg |
The decomposition temperature analysis of the hypo-aluminum orthophosphate that table 4 embodiment 2 and comparative example 1 make
Can see the hypo-aluminum orthophosphate that the granular size of the hypo-aluminum orthophosphate that the embodiment of the present invention 2 makes makes much smaller than prior art from table 3.The infrared detection collection of illustrative plates of Fig. 3 hypo-aluminum orthophosphate that to be embodiment 2 make with comparative example 1.The infared spectrum of the hypo-aluminum orthophosphate that the hypo-aluminum orthophosphate that embodiment 2 makes as can see from Figure 3 and comparative example 1 make is basic identical, and main absorption peak can be on deserved; The particle diameter of the hypo-aluminum orthophosphate making due to embodiment 2 is smaller, so the infrared absorption peak of the hypo-aluminum orthophosphate that embodiment 2 makes is eager to excel than comparative example 1.The hot weightless picture of Fig. 4 hypo-aluminum orthophosphate that to be embodiment 2 make with comparative example 1.The decomposition temperature that can see the hypo-aluminum orthophosphate that the embodiment of the present invention 1 makes from Fig. 4 and table 4 is greater than the hypo-aluminum orthophosphate that prior art makes.
Embodiment 3
A method of producing hypo-aluminum orthophosphate with reaction extrusion process, comprises the following steps:
(1) 3122g potassium hypophosphite and 1333g aluminum chloride are mixed, then compound being added to Temperature Setting is to react and extrude in the twin screw extruder of 60 ℃; Extrude and obtain white mud shape product through reaction;
(2) product of step (1) is preserved to slaking 12h at the environment lower seal of 60 ℃; Then by product washing, filtration and dry, obtain the hypo-aluminum orthophosphate of white powder.After testing, to obtain the productive rate of product be 98% to the present embodiment.The sreen analysis of the hypo-aluminum orthophosphate of gained is in table 5, and Fig. 5 is shown in by infrared detection collection of illustrative plates, and hot weightless picture is shown in Fig. 6 and table 6.
The sreen analysis of the hypo-aluminum orthophosphate that table 5 embodiment 3 and comparative example 1 make
| ? | Meso-position radius | Volume mean diameter | Area average diameter | Length mean diameter | Specific surface area |
| Embodiment 3 | 3.623μm | 6.042μm | 1.573μm | 0.392μm | 1291m^2/kg |
| Comparative example 1 | 24.61μm | 32.27μm | 10.31μm | 1.926μm | 215.3m^2/kg |
The decomposition temperature analysis of the hypo-aluminum orthophosphate that table 6 embodiment 3 and comparative example 1 make
Can see the hypo-aluminum orthophosphate that the granular size of the hypo-aluminum orthophosphate that the embodiment of the present invention 3 makes makes much smaller than prior art from table 5.The infrared detection collection of illustrative plates of Fig. 5 hypo-aluminum orthophosphate that to be embodiment 3 make with comparative example 1.The infared spectrum of the hypo-aluminum orthophosphate that the hypo-aluminum orthophosphate that embodiment 3 makes as can see from Figure 5 and comparative example 1 make is basic identical, and main absorption peak can be on deserved; The particle diameter of the hypo-aluminum orthophosphate making due to embodiment 3 is smaller, so the infrared absorption peak of the hypo-aluminum orthophosphate that embodiment 3 makes is eager to excel than comparative example 1.The hot weightless picture of Fig. 6 hypo-aluminum orthophosphate that to be embodiment 3 make with comparative example 1.The decomposition temperature that can see the hypo-aluminum orthophosphate that the embodiment of the present invention 3 makes from Fig. 6 and table 6 is greater than the hypo-aluminum orthophosphate that prior art makes.
Embodiment 4
A method of producing hypo-aluminum orthophosphate with reaction extrusion process, comprises the following steps:
(1) Hypophosporous Acid, 50 that is 50% by 3960g massfraction and 610g aluminum oxide mix, and then compound being added to Temperature Setting is to react and extrude in the twin screw extruder of 80 ℃; Extrude and obtain white mud shape product through reaction;
(2) product of step (1) is preserved to slaking 36h at the environment lower seal of 30 ℃; Then by product washing, filtration and dry, obtain the hypo-aluminum orthophosphate of white powder.After testing, to obtain the productive rate of product be 98% to the present embodiment.The sreen analysis of the hypo-aluminum orthophosphate of gained is in table 7, and Fig. 7 is shown in by infrared detection collection of illustrative plates, and hot weightless picture is shown in Fig. 8 and table 8.
The sreen analysis of the hypo-aluminum orthophosphate that table 7 embodiment 4 and comparative example 1 make
| ? | Meso-position radius | Volume mean diameter | Area average diameter | Length mean diameter | Specific surface area |
| Embodiment 4 | 3.362μm | 5.714μm | 1.384μm | 0.331μm | 1751m^2/kg |
| Comparative example 1 | 24.61μm | 32.27μm | 10.31μm | 1.926μm | 215.3m^2/kg |
The decomposition temperature analysis of the hypo-aluminum orthophosphate that table 8 embodiment 4 and comparative example 1 make
Can see the hypo-aluminum orthophosphate that the granular size of the hypo-aluminum orthophosphate that the embodiment of the present invention 4 makes makes much smaller than prior art from table 7.The infrared detection collection of illustrative plates of Fig. 7 hypo-aluminum orthophosphate that to be embodiment 4 make with comparative example 1.The infared spectrum of the hypo-aluminum orthophosphate that the hypo-aluminum orthophosphate that embodiment 4 makes as can see from Figure 7 and comparative example 1 make is basic identical, and main absorption peak can be on deserved; The particle diameter of the hypo-aluminum orthophosphate making due to embodiment 4 is smaller, so the infrared absorption peak of the hypo-aluminum orthophosphate that embodiment 4 makes is eager to excel than comparative example 1.The hot weightless picture of Fig. 8 hypo-aluminum orthophosphate that to be embodiment 4 make with comparative example 1.The decomposition temperature that can see the hypo-aluminum orthophosphate that the embodiment of the present invention 4 makes from Fig. 8 and table 8 is greater than the hypo-aluminum orthophosphate that prior art makes.
Embodiment 5
A method of producing hypo-aluminum orthophosphate with reaction extrusion process, comprises the following steps:
(1) Hypophosporous Acid, 50 that is 50% by 3960g massfraction and 780g aluminium hydroxide mix, and then compound being added to Temperature Setting is to react and extrude in the twin screw extruder of 40 ℃; Extrude and obtain white mud shape product through reaction;
(2) product of step (1) is preserved to slaking 48h at the environment lower seal of 20 ℃; Then by product washing, filtration and dry, obtain the hypo-aluminum orthophosphate of white powder.After testing, to obtain the productive rate of product be 98% to the present embodiment.The sreen analysis of the hypo-aluminum orthophosphate of gained is in table 9, and Fig. 9 is shown in by infrared detection collection of illustrative plates, and hot weightless picture is shown in Figure 10 and table 10.
The sreen analysis of the hypo-aluminum orthophosphate that table 9 embodiment 5 and comparative example 1 make
| ? | Meso-position radius | Volume mean diameter | Area average diameter | Length mean diameter | Specific surface area |
| Embodiment 5 | 3.471μm | 5.832μm | 1.492μm | 0.354μm | 1572m^2/kg |
| Comparative example 1 | 24.61μm | 32.27μm | 10.31μm | 1.926μm | 215.3m^2/kg |
The decomposition temperature analysis of the hypo-aluminum orthophosphate that table 10 embodiment 5 and comparative example 1 make
Can see the hypo-aluminum orthophosphate that the granular size of the hypo-aluminum orthophosphate that the embodiment of the present invention 5 makes makes much smaller than prior art from table 9.The infrared detection collection of illustrative plates of Fig. 9 hypo-aluminum orthophosphate that to be embodiment 5 make with comparative example 1.The infared spectrum of the hypo-aluminum orthophosphate that the hypo-aluminum orthophosphate that embodiment 5 makes as can see from Figure 9 and comparative example 1 make is basic identical, and main absorption peak can be on deserved; The particle diameter of the hypo-aluminum orthophosphate making due to embodiment 5 is smaller, so the infrared absorption peak of the hypo-aluminum orthophosphate that embodiment 5 makes is eager to excel than comparative example 1.The hot weightless picture of Figure 10 hypo-aluminum orthophosphate that to be embodiment 5 make with comparative example 1.The decomposition temperature that can see the hypo-aluminum orthophosphate that the embodiment of the present invention 5 makes from Figure 10 and table 10 is greater than the hypo-aluminum orthophosphate that prior art makes.
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 hypo-aluminum orthophosphate with reaction extrusion process, is characterized in that, comprises the following steps:
(1) by hypophosphite and aluminium salt, or Hypophosporous Acid, 50 and aluminium hydroxide, or Hypophosporous Acid, 50 and aluminum oxide, after mixing, on twin screw extruder, react and extrude;
(2) by the product of step (1) at 20～80 ℃ of slaking 4～48h; Then by product washing, filtration and dry, obtain described hypo-aluminum orthophosphate.
2. method according to claim 1, is characterized in that, it is 40～80 ℃ that the described twin screw extruder of step (1) reacts the temperature of extruding.
3. method according to claim 2, is characterized in that, the temperature that described reaction is extruded is 50 ℃.
4. method according to claim 1, is characterized in that, the described hypophosphite of step (1) is sodium hypophosphite, potassium hypophosphite or ammonium hypophosphite; Described aluminium salt is Tai-Ace S 150, aluminum chloride or aluminum nitrate.
5. method according to claim 1, is characterized in that, the described curing temperature of step (2) is 30～80 ℃.
6. method according to claim 5, is characterized in that, described curing temperature is 50～60 ℃.
7. method according to claim 1, is characterized in that, the described curing time of 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)
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| CN111961254A (en) * | 2020-08-27 | 2020-11-20 | 湖北航天化学技术研究所 | Preparation method of modified aluminum hypophosphite flame retardant |
| CN114772568A (en) * | 2021-09-30 | 2022-07-22 | 四川金核高分子材料有限公司 | Method for preparing modified aluminum hypophosphite and product thereof |
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Application publication date: 20140625 |