CN1073659A - The purifying method of yellow phosphorus - Google Patents
The purifying method of yellow phosphorus Download PDFInfo
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- CN1073659A CN1073659A CN 91111846 CN91111846A CN1073659A CN 1073659 A CN1073659 A CN 1073659A CN 91111846 CN91111846 CN 91111846 CN 91111846 A CN91111846 A CN 91111846A CN 1073659 A CN1073659 A CN 1073659A
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- yellow phosphorus
- phosphorus
- active carbon
- powdered active
- molten mass
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Abstract
Present method comprises in the yellow phosphorus molten mass adds specific surface area less than 800 meters
2The powdered active carbon of/gram, various components are mixed under turbulence state, and its time length should be enough to it is contacted, and the suspension that is generated is separated into purifies phosphorus and solid sediment, and the interpolation of various components and mix stages carry out in inert atmosphere.
Description
The present invention relates to the yellow phosphorus purification method, this phosphorus can be used for production foodstuffs industry as a kind of raw material, the pure especially material that radio industry and aircraft industry use.
The yellow phosphorus of producing with known certain methods contains a large amount of organic and inorganic impurity, especially carbide, metallic salt and metal oxide, and sulfide.The content (weight %) that relates to following impurity is purified the major requirement of phosphorus: organic impurity is no more than 0.003, and iron compound is converted into iron and is no more than 0.0005, and sulfide is converted into sulphur and is lower than 0.002.Undissolved residue (CS in the dithiocarbonic anhydride
2Middle H.O) content should not surpass 0.001%.
Known yellow phosphorus purification method (JP, B 49-9315), are that the yellow phosphorus molten mass is mixed with granular carbon in the presence of water, subsequently the mixed solution of making are heated to 98-102 ℃, again from the steam gas that forms mutually condensation go out phosphorus.
Aforesaid method is mainly effective to the organic compound of removing in the phosphorus, because the organic compound boiling point is higher, they remain in the liquid phase during phosphorus evaporation.
In above-mentioned flow process, because the existence of the water that high temperature and obstruction gac and phosphorus actively contact is to the detrimentally affect of charcoal adsorptivity, gac can not guarantee effectively to remove inorganic impurity.In addition, this technology has bigger fire, needs to adopt special corrosion resistant equipment, and being characterized in producing has a large amount of phosphorus-containing wastewaters and gaseous waste.
Method (the DE of the compound of iron, lead, arsenic in the known removing yellow phosphorus, B, 1143794) be that molten mass with phosphorus mixes with Tripyrophosphoric acid, from the emulsion that forms, separate acid, yellow phosphorus by the distillation tower of gac and kaolin mixture is housed, is then isolated the yellow phosphorus of purification.
Yellow phosphorus after the purification contains inorganic impurity 0.005%, organic impurity 0.009%.This method can not guarantee the high purification of phosphorus, need the refuse that contain a large amount of phosphorus be utilized, and is characterized in that current consumption is big.
Known yellow phosphorus purification method (DE, B, 2135546) be to add the gac aqeous suspension in the yellow phosphorus molten mass,, with separating method the suspension that forms be separated into the solid precipitation thing and contain organic impurity and be no more than 0.001% purification phosphorus by the counter-current principle intermingling.In purification,, adopt gac and unit surface to be not less than 800 meters according to 0.5～5% of phosphorus weight
2/ gram.Contacting of gac suspension and phosphorus is no more than the 0.5-15 branch, preferably phosphorus handled simultaneously secondary or more times, to improve degree of purification.
Aforesaid method can be removed the organic impurity in the phosphorus, to removing mineral compound, especially iron, sulphur compound poor effect.The selective adsorption capacity of gac is decided by (800 meters of bigger specific surface areas in this flow process
2/ gram), the hole shape structure of gac, the size of its hole is suitable with the molecular size of organic compound.Because mixing process is carried out in adverse current, the contacted deficiency of time of the aqeous suspension of phosphorus and gac is to adsorb mineral compound effectively.When the gac aqeous suspension of phosphorus and preparation again when repeatedly contacting, just can reach and highly remove organic impurity, the water resistance of filling hinders yellow phosphorus and contacts more energetically with gac in the gac hole.The characteristics of this method are that technology is simple, but produce the waste water that is polluted by phosphorus and charcoal are arranged in a large number, and this need append the expense of dephosphorization and carbon removal.
The present invention is based on following task: under the condition of using the gac of having chosen characteristic, develop a kind of by changing the method that various components introducings and hybrid mode purify yellow phosphorus, to guarantee highly to remove the organic and inorganic impurity in the yellow phosphorus, be characterized in that technology was both simple, economical again.
The terms of settlement of this task is to propose a kind of method that purifies yellow phosphorus, this method comprises in the molten mass of phosphorus adds gac and it is mixed formation suspension, then suspension is separated into the yellow phosphorus and the solid residue of purification, according to the present invention, in the yellow phosphorus molten mass, add Powdered specific surface area less than 800 meters
2The gac of/gram mixes under turbulence state, and its mixing time should be enough to make various components to contact, and interpolation and mixing step carry out in rare gas element.
The method of being recommended can guarantee to remove organic impurity in the yellow phosphorus and reach and be lower than 0.003%, inorganic impurity (weight %): iron compound, and be converted into iron and reach 0.0005%, sulfide is converted into sulphur and reaches 0.0008%, and undissolved residue 0.001% in the dithiocarbonic anhydride.High like this degree of purification is by guaranteeing that specific surface area is less than 800 meters
2The charcoal absorption decision of/gram, the structure of this gac has formed macrovoid and ultramicropore.The latter plays a part to transmit passage and suitable with the molecular size of inorganic impurity, thereby has guaranteed active adsorption all dirt equably.
Recommend to use the powdered active carbon of from semicoke or peat, producing.This gac has optimum performance aspect specific surface area.Add the preferably 3-5% of phosphorus weight of charcoal amount, degree of purification is lowered because be less than 3%, overweight 5% owing to lack influence, poor effect to degree of purification.
The mixing step that carries out under turbulence state to the degree of purification influence greatly.In this state, form the equally distributed suspension of gac, at this moment cause various component contacts and improve gac adsorbs impurity from yellow phosphorus optimum conditions along the whole volume of yellow phosphorus.
Re remains on 1 * 10 when number
5To 5 * 10
6During scope, remove organic and best results inorganic impurity, depend on the weight and the turbulence state condition of component the duration of contact of gac and phosphorus, the suggestion mixing time continues 20-60 minute, and this purifies the yellow phosphorus of any amount effectively with regard to being enough to.
Because the yellow phosphorus spontaneous ignition temperature is low, contact with oxygen for preventing phosphorus, the suggestion component adds and mixing step carries out in inert atmosphere, for example carries out in nitrogen, carbonic anhydride.For the phosphorus of isolation of purified, the suggestion under the pressure that is not higher than 0.4 MPa with suspension filtered, transition band left the solid precipitation thing, wherein 70 weight % are by the gac of contaminating impurity, about 30 weight % are yellow phosphorus.Broken these solid precipitation things of the most handy vibratory drilling method when pressure surpasses 0.4 MPa, are difficult to scavenger precipitation thing from transition band.
Because the method for being recommended directly makes an addition to powdery carbon in yellow phosphorus in inert environments, saved preparation gac aqeous suspension step, thereby reduced the toxic waste amount and in high purification, improved the economy of process.
Enumerate some specific exampless that present method is implemented below according to the present invention.
Embodiment 1
Sending into foreign matter content (weight %) in the container of the belt stirrer of rare gas element-nitrogen abrim is: organism 0.19, iron compound 0.02, sulfide 0.004,100 of the undissolved residue 0.1 3 gram powdered active carbons that restrain the molten yellow phosphorus and make with semicoke in the dithiocarbonic anhydride, its specific surface area is 100 meters
2/ gram.Various components mix under turbulence state, and its Re number equals 1 * 10
5, 20 minutes time length.Obtained suspension is separated into the yellow phosphorus and the solid sediment-filter cake of purification after filtration in strainer under 0.3 MPa, for from strainer, removing filter cake, with vibratory drilling method with its fragmentation.
Yellow phosphorus impure (weight %): organism is lower than 0.003, iron cpd 0.0006, and sulfide 0.001, undissolved residue 0.001 in the dithiocarbonic anhydride.
Embodiment 2
Sending into foreign matter content in the container of the band stirrer of rare gas element-carbonic anhydride abrim is: organism 0.19, iron compound 0.02, sulfide 0.004,100 of undissolved residue 0.01 gram molten yellow phosphorus and make in the dithiocarbonic anhydride with peat, specific surface area is 700 meters
2The powdered active carbon of/gram.Various components are under turbulence state, and the Re number equals 5 * 10
6Shi Jinhang mixes, and the time length is 60 minutes.Obtained suspension becomes the yellow phosphorus and the solid sediment-filter cake of purification through the filter filtering separation under 0.4 MPa pressure.For from strainer, removing filter cake, with vibratory drilling method with its fragmentation.
Yellow phosphorus impure (weight %): organism is lower than 0.003, iron compound 0.0005, and sulfide 0.0008, undissolved residue is lower than 0.001 in the dithiocarbonic anhydride.
Embodiment 3
Sending into foreign matter content (weight %) in the container of the band stirrer that is full of rare gas element-nitrogen is: organism 0.19, iron cpd 0.02, sulfide 0.004,100 of undissolved residue 0.01 gram molten yellow phosphorus and make in the dithiocarbonic anhydride with semicoke, specific surface area is 400 meters
24 gram powdered active carbons of/gram.Various components are under turbulence state, and the Re number equals 5 * 10
5Shi Jinhang mixes, 40 minutes time length.Obtained suspension becomes to purify yellow phosphorus and solid sediment-filter cake through filtering separation in the filter under 0.2 MPa pressure, for from strainer, removing filter cake, with vibratory drilling method with its fragmentation.
Yellow phosphorus impure (weight %): organism is lower than 0.003, iron compound 0.0005, and sulfide 0.0009, undissolved residue is lower than 0.001 in the dithiocarbonic anhydride.
Claims (7)
1, yellow phosphorus purification method, this method comprise in the yellow phosphorus molten mass adds gac, mixes the back and generates suspension, then with its yellow phosphorus and solid sediment that is separated into purification, is characterized in: add specific surface area less than 800 meters in the yellow phosphorus molten mass
2The powdered active carbon of/gram, mixing is carried out under turbulent flow conditions, and the time length should be enough to make various components to contact, and interpolation and mixing step carry out in inert atmosphere;
2, the method for claim 1 is characterized in that using the powdered active carbon with semicoke or peat preparation;
3, claim 1,2 method, the quantity that it is characterized in that adding powdered active carbon is the 3-5% of yellow phosphorus weight;
4, the method for claim 1 is characterized in that yellow phosphorus molten mass and powdered active carbon mix under turbulent flow conditions, its Re number equals 1 * 10
5-5 * 10
6;
5, claim 1,4 method is characterized in that yellow phosphorus molten mass and powdered active carbon mixed duration are 20-60 minute;
6, the method for claim 1 is characterized in that using nitrogen and carbonic anhydride as rare gas element;
7, the method for claim 1 is characterized in that under the pressure that is no more than 0.4 MPa, purifies phosphorus and solid sediment by filtering suspension is separated into, then with vibratory drilling method with the solid sediment fragmentation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 91111846 CN1073659A (en) | 1991-12-23 | 1991-12-23 | The purifying method of yellow phosphorus |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 91111846 CN1073659A (en) | 1991-12-23 | 1991-12-23 | The purifying method of yellow phosphorus |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1073659A true CN1073659A (en) | 1993-06-30 |
Family
ID=4910896
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 91111846 Pending CN1073659A (en) | 1991-12-23 | 1991-12-23 | The purifying method of yellow phosphorus |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1073659A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101759164B (en) * | 2009-12-09 | 2011-08-10 | 湖北兴福电子材料有限公司 | Production method of high-purity yellow phosphorus |
| CN103588185A (en) * | 2013-11-14 | 2014-02-19 | 云南江磷集团股份有限公司 | Method for removing sulfur from yellow phosphorus |
| CN109562943A (en) * | 2016-08-08 | 2019-04-02 | 朗盛德国有限责任公司 | Method for purifying yellow phosphorus |
-
1991
- 1991-12-23 CN CN 91111846 patent/CN1073659A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101759164B (en) * | 2009-12-09 | 2011-08-10 | 湖北兴福电子材料有限公司 | Production method of high-purity yellow phosphorus |
| CN103588185A (en) * | 2013-11-14 | 2014-02-19 | 云南江磷集团股份有限公司 | Method for removing sulfur from yellow phosphorus |
| CN103588185B (en) * | 2013-11-14 | 2016-03-02 | 云南江磷集团股份有限公司 | Yellow phosphorus sulfur method |
| CN109562943A (en) * | 2016-08-08 | 2019-04-02 | 朗盛德国有限责任公司 | Method for purifying yellow phosphorus |
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| C01 | Deemed withdrawal of patent application (patent law 1993) | ||
| WD01 | Invention patent application deemed withdrawn after publication |