CN102303849A - Method for preparing high-purity boron nitride - Google Patents
Method for preparing high-purity boron nitride Download PDFInfo
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- CN102303849A CN102303849A CN201110238620A CN201110238620A CN102303849A CN 102303849 A CN102303849 A CN 102303849A CN 201110238620 A CN201110238620 A CN 201110238620A CN 201110238620 A CN201110238620 A CN 201110238620A CN 102303849 A CN102303849 A CN 102303849A
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Abstract
The invention relates to a method for preparing high-purity boron nitride, which comprises the following steps: (1) placing analytically pure urea into an evaporation pan, adding distillated water, dissolving, filtering, heating the filtrate, concentrating, cooling, crystallizing and obtaining pure urea crystals; (2) placing analytically pure boric acid into the evaporation pan, adding distilled water, dissolving, filtering, heating the filtrate, concentrating, cooling, crystallizing and obtaining pure boric acid crystals; and (3) mixing the purified urea crystals and boric acid crystals, heating, introducing nitrogen, rising the temperature to 160 to 170 DEG C, curing, continuing to rise the temperature, volatilizing, cooling, taking out, grinding into fine powder, calcining under a condition of introducing nitrogen, cooling and obtaining high-purity boron nitride. The method for preparing high-purity boron nitride, which is disclosed by the invention, synthesizes boron nitride by purifying urea and boric acid and synthesizing. The method can prepare high-purity boron nitride and is simple and low in cost, and the operation of the method is easy.
Description
Technical field:
The present invention relates to mineral compound preparation method field, particularly a kind of preparation method of high-purity SP 1.
Background technology:
High-purity SP 1 is corrosion-resistant, and electrical insulating property is fine, is widely used in semi-conductive solid doped technology; Semi-conductor is used wrapping material with anti-neutron radiation in high-temperature material, the instrument; High temperature solid lubricant; The special electrolysis of the condition of high temperature, resistive material; Be pressed into different shape; Be used as high temperature, high pressure, insulation, thermal component.
Present preparation method is: fusion and the boron trioxide of pulverizing and urea mixing; Place porcelain crucible heating, calcination; Make SP 1, the SP 1 purity that this kind method is produced is low, productive rate is low, foreign matter content is high, can not satisfy high request product demand in the electronic industry.
Summary of the invention:
The objective of the invention is to overcome the deficiency of prior art, provide that a kind of purity is high, foreign matter content is low, process step is simple, productive rate is high, the preparation method of high-purity SP 1.
The present invention realizes through following technical scheme:
A kind of preparation method of high-purity SP 1 the steps include:
(1) purification urea
Analytical pure urea is put into furnace pot, add 75-85 ℃ of zero(ppm) water heating, after the molten appearance, filter; Filtrating is poured in the furnace pot, and heating concentrates, and temperature is 180-190 ℃; Concentrated density is controlled at 18-22Be, stops heating, crystallisation by cooling, the urea crystals that must purify;
The weight ratio of described analytical pure urea and zero(ppm) water is 2: 1;
(2) purification boric acid
Analytical pure boric acid is put into furnace pot, add 65-75 ℃ of zero(ppm) water heating, after the molten appearance, filter; Filtrating is poured in the furnace pot, and heating concentrates, and temperature is 175-185 ℃; Concentrated density is controlled at 19-21Be, stops heating, crystallisation by cooling, the boric acid crystallization that must purify;
Described analytical pure boric acid and zero(ppm) water weight ratio are 1: 4;
(3) synthetic high-purity SP 1
With the boric acid crystallization that the urea crystals and the step (2) of step (1) purification are purified, be mixing in 2: 1 according to weight ratio, under 60-65 ℃ of temperature, heat, begin fusion, be transparence; Feed nitrogen, reaction 1.5-2h, slowly elevated temperature solidifies to 160-170 ℃ again; Continue to be warming up to 320-350 ℃, behind the volatilization 2-3h, stop heating, cooling is taken out, the porphyrize powdery, and in the quartz boat of packing into, boat is placed in the silica tube; Under logical nitrogen situation, in 950-1000 ℃, behind the calcining 5-6h, in stream of nitrogen gas, cool off room temperature, promptly get high-purity SP 1.
And furnace pot is an evaporating dish in said step (1), (2).
And the urea crystals of purifying in the said step (3) and the boric acid crystallization of purification are packed in the three-necked flask, and on electric furnace, heat.
Advantage of the present invention and beneficial effect are:
1, the preparation method of the high-purity SP 1 of the present invention adopts purification urea and boric acid, synthetic high-purity SP 1, and this method can access the high SP 1 of purity, and the preparation method is simple, lower, the processing ease of cost.
2, foreign matter content of the present invention is low, purity is high, productive rate is high, production technique is advanced, simple, be the preparation method of the higher high-purity SP 1 of a kind of production efficiency.
Embodiment:
Do further detailed description below in conjunction with embodiment, following examples are descriptive, are not determinate, can not limit protection scope of the present invention with this.
Embodiment 1
A kind of preparation method of high-purity SP 1 the steps include:
(1) purification urea
1Kg analytical pure urea is put into evaporating dish, adds zero(ppm) water 500ml, heat 80 ℃ dissolve appearance after, filtration; Then filtrating is poured in the evaporating dish, heating concentrates, 185 ℃ of temperature; Concentrated density is controlled at 20Be, stops heating, and the urea crystals after crystallisation by cooling obtains purifying is subsequent use.
(2) purification boric acid
0.5Kg analytical pure boric acid is put into evaporating dish, add zero(ppm) water 2000ml, be heated to 65 ℃, after the molten appearance; Filter, then filtrating is poured in the evaporating dish, heating concentrates; 180 ℃ of concentrated density of temperature are controlled at 20Be, stop heating, and the boric acid crystallization after crystallisation by cooling obtains purifying is subsequent use.
(1) becomes high-purity SP 1
With the urea 500g after step (1) purification, and the boric acid crystallization after step (2) purification, 250g is in the three-necked flask of packing into; On electric furnace, be heated to 60 ℃, the beginning fusion is transparence; Feed nitrogen, take away the moisture content in the reaction solution, time 1.5h; Elevated temperature to 160 ℃ slowly again, this moment, hyalosome bleached, and solidified; Continue to be warming up to 330 ℃, this moment, a large amount of urea decomposition ammonia volatilizations were walked; Behind the volatilization 2h, stop heating, cooling is taken out, the porphyrize powdery, and in the quartz boat of packing into, boat is placed in the silica tube; Under logical nitrogen situation, in 950 ℃ of calcination 5h, in stream of nitrogen gas, cool off room temperature then, take out and obtain high-purity SP 1.
Embodiment 2
A kind of preparation method of high-purity SP 1 the steps include:
(1) pure urea
1.2Kg analytical pure urea is put into evaporating dish, add zero(ppm) water 600ml, heating, 75 ℃; The dissolving after-filtration is poured filtrating in the evaporating dish into then, and heating concentrates, and temperature is 180 ℃; Concentrated density is controlled at 22Be, stops heating, crystallisation by cooling, the urea crystals after obtaining purifying;
(2) pure boric acid
0.6Kg analytical pure boric acid is put into evaporating dish, add zero(ppm) water 2400ml, heat 75 ℃, the dissolving after-filtration; Then filtrating is poured in the evaporating dish, heating concentrates, 175 ℃ of temperature, and concentrated density is controlled at 21Be; Stop heating, crystallisation by cooling, the boric acid crystallization after obtaining purifying;
(3) become high-purity SP 1
Boric acid crystallization 300g with after urea 600g after step (1) purification and step (2) purification is contained in the three-necked flask, and heating is 65 ℃ on electric furnace; The beginning fusion is transparence, feeds nitrogen; Take away the moisture content in the reaction, time 2h, elevated temperature to 170 ℃ slowly again; This moment, hyalosome bleached, and solidified; Continue to be warming up to 320 ℃, this moment, a large amount of urea decomposition ammonia volatilizations went out, and behind the volatilization 3h, stopped heating; Cooling is taken out, and the porphyrize powdery is in the quartz boat of packing into; Boat is placed in the silica tube, under logical nitrogen situation, in 1000 ℃ of calcination 6h, in nitrogen gas stream, cools off room temperature then, takes out to obtain high-purity SP 1.
Claims (3)
1. the preparation method of a high-purity SP 1, be characterised in that: preparing method's concrete steps are:
(1) purification urea
Analytical pure urea is put into furnace pot, add 75-85 ℃ of zero(ppm) water heating, after the molten appearance, filter; Filtrating is poured in the furnace pot, and heating concentrates, and temperature is 180-190 ℃; Concentrated density is controlled at 18-22Be, stops heating, crystallisation by cooling, the urea crystals that must purify;
The weight ratio of described analytical pure urea and zero(ppm) water is 2: 1;
(2) purification boric acid
Analytical pure boric acid is put into furnace pot, add 65-75 ℃ of zero(ppm) water heating, after the molten appearance, filter; Filtrating is poured in the furnace pot, and heating concentrates, and temperature is 175-185 ℃; Concentrated density is controlled at 19-21Be, stops heating, crystallisation by cooling, the boric acid crystallization that must purify;
Described analytical pure boric acid and zero(ppm) water weight ratio are 1: 4;
(3) synthetic high-purity SP 1
With the boric acid crystallization that the urea crystals and the step (2) of step (1) purification are purified, be mixing in 2: 1 according to weight ratio, under 60-65 ℃ of temperature, heat, begin fusion, be transparence; Feed nitrogen, reaction 1.5-2h, slowly elevated temperature solidifies to 160-170 ℃ again; Continue to be warming up to 320-350 ℃, behind the volatilization 2-3h, stop heating, cooling is taken out, the porphyrize powdery, and in the quartz boat of packing into, quartz boat is placed in the silica tube; Under logical nitrogen situation, in 950-1000 ℃, behind the calcining 5-6h, in stream of nitrogen gas, cool off room temperature, promptly get high-purity SP 1.
2. the preparation method of high-purity SP 1 according to claim 1 is characterized in that: furnace pot is an evaporating dish in said step (1), (2).
3. the preparation method of high-purity SP 1 according to claim 1 is characterized in that: the urea crystals of purifying in the said step (3) and the boric acid crystallization of purification are packed in the three-necked flask, and on electric furnace, heat.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103864029A (en) * | 2014-03-28 | 2014-06-18 | 武汉科技大学 | Hexagonal boron nitride powder and preparation method of hexagonal boron nitride |
| CN105293453A (en) * | 2015-11-20 | 2016-02-03 | 汕头大学 | Doped hexagonal boron nitride nano sheet, preparation method thereof, catalyst using same as carrier, and applications thereof |
| CN106140240A (en) * | 2015-04-24 | 2016-11-23 | 中国科学院金属研究所 | A kind of low-carbon alkanes or alkylbenzene oxidative dehydrogenation boron nitride catalyst and its preparation method and application |
| CN108384983A (en) * | 2018-03-06 | 2018-08-10 | 浙江灿根智能科技有限公司 | A kind of high-strength copper based alloy material |
| CN109019534A (en) * | 2018-09-29 | 2018-12-18 | 西南石油大学 | A kind of preparation method of ultrathin boron nitride nanosheet |
| CN112724787A (en) * | 2021-01-07 | 2021-04-30 | 江南大学 | Preparation method of polyaniline modified graphene oxide/hydroxylated boron nitride composite epoxy coating |
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2011
- 2011-08-19 CN CN201110238620A patent/CN102303849A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103864029A (en) * | 2014-03-28 | 2014-06-18 | 武汉科技大学 | Hexagonal boron nitride powder and preparation method of hexagonal boron nitride |
| CN103864029B (en) * | 2014-03-28 | 2016-01-13 | 武汉科技大学 | A kind of hexagonal boron nitride powder preparation method |
| CN106140240A (en) * | 2015-04-24 | 2016-11-23 | 中国科学院金属研究所 | A kind of low-carbon alkanes or alkylbenzene oxidative dehydrogenation boron nitride catalyst and its preparation method and application |
| CN106140240B (en) * | 2015-04-24 | 2018-11-13 | 中国科学院金属研究所 | A kind of low-carbon alkanes or alkylbenzene oxidative dehydrogenation nitridation B catalyst and its preparation method and application |
| CN105293453A (en) * | 2015-11-20 | 2016-02-03 | 汕头大学 | Doped hexagonal boron nitride nano sheet, preparation method thereof, catalyst using same as carrier, and applications thereof |
| CN105293453B (en) * | 2015-11-20 | 2018-05-11 | 汕头大学 | It is a kind of to adulterate hexagonal boron nitride nanosheet and preparation method thereof and using its catalyst and application as carrier |
| CN108384983A (en) * | 2018-03-06 | 2018-08-10 | 浙江灿根智能科技有限公司 | A kind of high-strength copper based alloy material |
| CN109019534A (en) * | 2018-09-29 | 2018-12-18 | 西南石油大学 | A kind of preparation method of ultrathin boron nitride nanosheet |
| CN112724787A (en) * | 2021-01-07 | 2021-04-30 | 江南大学 | Preparation method of polyaniline modified graphene oxide/hydroxylated boron nitride composite epoxy coating |
| CN112724787B (en) * | 2021-01-07 | 2022-06-28 | 江南大学 | Preparation method of polyaniline modified graphene oxide/hydroxylated boron nitride composite epoxy coating |
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Application publication date: 20120104 |