CN103172086A - Phase stabilized ammonium nitrate additive and preparation method of phase stabilized ammonium nitrate - Google Patents
Phase stabilized ammonium nitrate additive and preparation method of phase stabilized ammonium nitrate Download PDFInfo
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Abstract
本发明公开了一种相稳定硝酸铵添加剂及其相稳定硝酸铵的制备方法，所述添加剂为2,3-二羟甲基-2,3-二硝基-1,4-丁二醇四月桂酸酯(BHDBTL)、2,3-二羟甲基-2,3-二硝基-1,4-丁二醇四棕榈酸酯(BHDBTP)或2,3-二羟甲基-2,3-二硝基-1,4-丁二醇四硬脂酸酯(BHDBTS)。相稳定硝酸铵的制备方法为：将烘干研磨粉碎过筛后的硝酸铵加入氯仿中，添加剂的加入量分别为硝酸铵质量分数的1~3%，搅拌，回流0.5h，减压蒸馏，过滤后干燥，将其研磨后过筛，再烘干至恒重。本发明采用的添加剂与普通的有机物改性剂相比，分子结构中均含有两个硝基，用其制备的相稳定硝酸铵的性能会有一定的改善。当添加量为1%-3%时，均有抑制硝酸铵Ⅲ~Ⅱ相转变的效果，且BHDBTP、BHDBTS对硝酸铵改性的效果要优于BHDBTL。
The invention discloses a phase-stabilized ammonium nitrate additive and a preparation method thereof. The additive is 2,3-dimethylol-2,3-dinitro-1,4-butanediol tetra Laurate (BHDBTL), 2,3-Dihydroxymethyl-2,3-dinitro-1,4-butanediol tetrapalmitate (BHDBTP) or 2,3-Dihydroxymethyl-2, 3-Dinitro-1,4-butanediol tetrastearate (BHDBTS). The preparation method of phase-stabilized ammonium nitrate is: add the ammonium nitrate after drying, grinding, pulverizing and sieving into chloroform, the addition amount of additives is 1-3% of the mass fraction of ammonium nitrate respectively, stir, reflux for 0.5h, and distill under reduced pressure, After filtering and drying, it was ground, sieved and dried to constant weight. Compared with common organic modifiers, the additive used in the present invention contains two nitro groups in the molecular structure, and the performance of the phase-stable ammonium nitrate prepared by using it will be improved to a certain extent. When the addition amount is 1%-3%, both have the effect of inhibiting the phase transformation of ammonium nitrate Ⅲ~Ⅱ, and the effect of BHDBTP and BHDBTS on the modification of ammonium nitrate is better than that of BHDBTL.
Description
Technical field
The present invention relates to the preparation method of a kind of phase stable ammonium nitrate additive and phase stable ammonium nitrate thereof, belong to the applied chemistry field.
Background technology
Ammonium nitrate (AN) is one of the domestic and international industrial explosive that generally adopts and oxygenant of solid propellant.But there is stable crystal formation on five kinds of thermodynamics in ammonium nitrate under normal pressure, and every kind of crystal formation only exists in certain temperature range.When becoming another kind of crystalline form by a kind of crystal phase transition, volume will be along with crystalline structure and lattice volume and is changed.This phase transition phenomenon is unfavorable for the use of ammonium nitrate, if temperature generating period variation, energy and crystalline density volume also can change thereupon, this variation is particularly evident in room temperature range, so that the interior cohesive force of ammonium nitrate changes, long storage time is more easily lumpd, and has affected the use of ammonium nitrate.To be mutually related between the polycrystallinity of ammonium nitrate itself, water absorbability and anti-caking three.The existence of a small amount of moisture is that the brilliant essential condition that becomes occurs ammonium nitrate, after the ammonium nitrate moisture absorption, the salt bridge that will form between adjacent particles, make nitric acid by particle tightly combine, cause serious caking.If the variation of temperature generating period, also can cause the volume of ammonium nitrate powder column constantly to change and degradation, affect the solid propellant made take ammonium nitrate as main raw material and the blast performance of industrial explosive, caused AN to be restricted in the application in industrial explosive and propelling agent field.Therefore, take effective measures and suppress or prevent that ammonium nitrate from occuring in the use temperature scope to change mutually that namely to prepare mutually stable ammonium nitrate be very necessary.
During phase stable ammonium nitrate, phase stabilization additives commonly used has inorganic salt or metal oxide, tensio-active agent and polymkeric substance etc. in preparation, but crosses polymictic introducing, can reduce the purity of ammonium nitrate, also can on incur loss.
Summary of the invention
The object of the present invention is to provide a kind of can suppress that ammonium nitrate II～III changes mutually 2,3-dihydroxymethyl-2, the fatty acid ester compound of 3-dinitrobenzene-BDO is as the preparation method of phase stabilization additives and phase stable ammonium nitrate thereof.
The technical scheme that realizes the object of the invention is: a kind of phase stable ammonium nitrate additive, described additive is 2,3-dihydroxymethyl-2,3-dinitrobenzene-1,4-butyleneglycol four laurates (BHDBTL), 2,3-dihydroxymethyl-2,3-dinitrobenzene-BDO four cetylates (BHDBTP) or 2,3-dihydroxymethyl-2,3-dinitrobenzene-BDO tetrastearate (BHDBTS), described additive add-on is 1 ~ 3% of ammonium nitrate massfraction.
A kind of preparation method of phase stable ammonium nitrate comprises the following steps:
Oven dry is ground ammonium nitrate, 2 after sieving, 3-dihydroxymethyl-2, the fatty acid ester compound of 3-dinitrobenzene-BDO adds in chloroform, fully stirs, and refluxes, and is dry after underpressure distillation is filtered, and it sieved after grinding, then dry to constant weight.
Described compound is 2,3-dihydroxymethyl-2,3-dinitrobenzene-BDO four laurates (BHDBTL), 2,3-dihydroxymethyl-2,3-dinitrobenzene-1,4-butyleneglycol four cetylates (BHDBTP) or 2,3-dihydroxymethyl-2,3-dinitrobenzene-1,4-butyleneglycol tetrastearate (BHDBTS), the addition of described additive are 1 ~ 3% of ammonium nitrate massfraction.
The particle diameter of described ammonium nitrate is 40 ~ 60 orders.
1. compare with common organic modifier, BHDBTL, BHDBTP and BHDBTS are that molecular structure is symmetrical and all contain the fatty acid ester of two nitros, can have some improvement with the performance of the phase stable ammonium nitrate of its preparation.
2. all contain polar group carbonyl and nitro in BHDBTL, BHDBTP and BHDBTS molecular structure, by electrostatic interaction can with the ammonium nitrate molecule in ionic bond, make the brilliant temperature rising of phase stable ammonium nitrate or enthalpy change reduce, brilliant parameter is reduced.
3. when addition is 1%-3%, the effect that BHDBTL has inhibition ammonium nitrate III ~ II to change mutually when the BHDBTL addition is 1%, 2%, makes ammonium nitrate III ~ II phase transition temperature be increased to respectively 92.08 ℃, 93.22 ℃, when addition is 3%, make the crystalline substance of III ~ II become the peak disappearance.
4. when the BHDBTP addition is 1%-3%, make the crystalline substance of ammonium nitrate III ~ II become the peak disappearance, all have and suppress the effect that ammonium nitrate III ~ II changes mutually.
5. when the BHDBTS addition is 1%-3%, make the crystalline substance of ammonium nitrate III ~ II become the peak disappearance, all have and suppress the effect that ammonium nitrate III ~ II changes mutually.
Description of drawings
Fig. 1 is the DSC curve of embodiment 1 BHDBTL phase stable ammonium nitrate.
Fig. 2 is the DSC curve of embodiment 2 BHDBTL phase stable ammonium nitrates.
Fig. 3 is the DSC curve of embodiment 3 BHDBTL phase stable ammonium nitrates.
Fig. 4 is the DSC curve of embodiment 4 BHDBTP phase stable ammonium nitrates.
Fig. 5 is the DSC curve of embodiment 5 BHDBTP phase stable ammonium nitrates.
Fig. 6 is the DSC curve of embodiment 6 BHDBTP phase stable ammonium nitrates.
Fig. 7 is the DSC curve of embodiment 7 BHDBTS phase stable ammonium nitrates.
Fig. 8 is the DSC curve of embodiment 8 BHDBTS phase stable ammonium nitrates.
Fig. 9 is the DSC curve of embodiment 9 BHDBTS phase stable ammonium nitrates.
Embodiment
The preparation of BHDBTL phase stable ammonium nitrate
After ammonium nitrate water recrystallization and be dried to constant weight.The ammonium nitrate that 20g ammonium nitrate oven dry is ground after sieve (60 order) adds in the chloroform of 30mL, adds 0.2g BHDBTL, stirs, backflow 0.5h, underpressure distillation, dry after filtering, sieve in (60 order) after it is ground, dry to constant weight under 80 ℃.Obtain the ammonium nitrate AN of BHDBTL modification
1
When table 1 is 1% when addition, the DSC data of BHDBTL phase stable ammonium nitrate
The preparation of BHDBTL phase stable ammonium nitrate
After ammonium nitrate water recrystallization and be dried to constant weight.The ammonium nitrate that 20g ammonium nitrate oven dry is ground after sieve (50 order) adds in the chloroform of 30mL, adds 0.4g BHDBTL, stirs, backflow 0.5h, underpressure distillation, dry after filtering, sieve in (50 order) after it is ground, dry to constant weight under 80 ℃.Obtain the ammonium nitrate AN of BHDBTL modification
2
When table 2 is 2% when addition, the DSC data of BHDBTL phase stable ammonium nitrate
Embodiment 3
The preparation of BHDBTL phase stable ammonium nitrate
After ammonium nitrate water recrystallization and be dried to constant weight.The ammonium nitrate that 20g ammonium nitrate oven dry is ground after sieve (40 order) adds in the chloroform of 30mL, adds 0.6g BHDBTL, stirs, backflow 0.5h, underpressure distillation, dry after filtering, sieve in (40 order) after it is ground, dry to constant weight under 80 ℃.Obtain the ammonium nitrate AN of BHDBTL modification
3
When table 3 is 3% when addition, the DSC data of BHDBTL phase stable ammonium nitrate
By embodiment 1,2,3 as can be known, when addition is 1%, in the time of 2% and 3%, the effect that BHDBTL has inhibition ammonium nitrate III ~ II to change mutually is when addition is 1%, 2%, make III ~ II phase transition temperature be increased to respectively 92.08 ℃, 93.22 ℃, when addition is 3%, make the crystalline substance of III ~ II become the peak disappearance, effect is relatively better.
The preparation of BHDBTP phase stable ammonium nitrate
After ammonium nitrate water recrystallization and be dried to constant weight.The ammonium nitrate that 20g ammonium nitrate oven dry is ground after sieve (60 order) adds in the chloroform of 30mL, adds 0.2g BHDBTP, stirs, backflow 0.5h, underpressure distillation, dry after filtering, sieve in (60 order) after it is ground, dry to constant weight under 80 ℃.Obtain the ammonium nitrate AN of BHDBTP modification
4
When table 4 is 1% when addition, the DSC data of BHDBTP phase stable ammonium nitrate
Embodiment 5
The preparation of BHDBTP phase stable ammonium nitrate
After ammonium nitrate water recrystallization and be dried to constant weight.The ammonium nitrate that 20g ammonium nitrate oven dry is ground after sieve (60 order) adds in the chloroform of 30mL, adds 0.4g BHDBTP, stirs, backflow 0.5h, underpressure distillation, dry after filtering, sieve in (60 order) after it is ground, dry to constant weight under 80 ℃.Obtain the ammonium nitrate AN of BHDBTP modification
5
When table 5 is 2% when addition, the DSC data of BHDBTP phase stable ammonium nitrate
The preparation of BHDBTP phase stable ammonium nitrate
After ammonium nitrate water recrystallization and be dried to constant weight.The ammonium nitrate that the oven dry of 20g ammonium nitrate is ground sieve rear (60 order) adds in the chloroform of 30mL, adds 0.6g BHDBTP, stirs, backflow 0.5h, underpressure distillation, dry after filtering, after it is ground, (60 order) sieves, and dries to constant weight under 80 ℃.Obtain the ammonium nitrate AN of BHDBTP modification
6
When table 6 is 3% when addition, the DSC data of BHDBTP phase stable ammonium nitrate
By embodiment 4,5,6 as can be known, and when the BHDBTP addition was 1%, 2%, 3%, the crystalline substance of III ~ II became the peak and disappears, and all has and suppress the effect that ammonium nitrate III ~ II changes mutually.
Embodiment 7
The preparation of BHDBTS phase stable ammonium nitrate
After ammonium nitrate water recrystallization and be dried to constant weight.The ammonium nitrate that 20g ammonium nitrate oven dry is ground after sieve (60 order) adds in the chloroform of 30mL, adds 0.2g BHDBTS, stirs, backflow 0.5h, underpressure distillation, dry after filtering, sieve in (60 order) after it is ground, dry to constant weight under 80 ℃.Obtain the ammonium nitrate AN of BHDBTS modification
7
When table 7 is 1% when addition, the DSC data of BHDBTS phase stable ammonium nitrate
The preparation of BHDBTS phase stable ammonium nitrate
With after ammonium nitrate water recrystallization and be dried to constant weight.The ammonium nitrate that 20g ammonium nitrate oven dry is ground after sieve (60 order) adds in the chloroform of 30mL, adds 0.4g BHDBTS, stirs, backflow 0.5h, underpressure distillation, dry after filtering, sieve in (60 order) after it is ground, dry to constant weight under 80 ℃.Obtain the ammonium nitrate AN of BHDBTS modification
8
When table 8 is 2% when addition, the DSC data of BHDBTS modified phase stable ammonium nitrate
Embodiment 9
The preparation of BHDBTS phase stable ammonium nitrate
After ammonium nitrate water recrystallization and be dried to constant weight.The ammonium nitrate that 20g ammonium nitrate oven dry is ground after sieve (60 order) adds in the chloroform of 30mL, adds 0.6g BHDBTS, stirs, backflow 0.5h, underpressure distillation, dry after filtering, sieve in (60 order) after it is ground, dry to constant weight under 80 ℃.Obtain the ammonium nitrate AN of BHDBTS modification
9
When table 9 is 3% when addition, the DSC data of BHDBTS phase stable ammonium nitrate
By embodiment 7,8,9 as can be known, and when addition was 1%, 2%, 3%, the crystalline substance of III ~ II became the peak and disappears, the effect that BHDBTS all has inhibition ammonium nitrate III ~ II to change mutually.
Additive B HDBTL, BHDBTP, BHDBTS when addition is 1%, 2%, 3%, all has and suppress the effect that ammonium nitrate III ~ II changes mutually, and BHDBTP, BHDBTS are better than BHDBTL to the effect of modification of ammonium nitrate.
Claims (5)
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Cited By (4)
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| CN103641670A (en) * | 2013-12-13 | 2014-03-19 | 南京理工大学 | Method for coating RDX cyclotrimethylene trinitramine and HMX cyclotetramethylene tetranitramine and coating material thereof |
| CN103641723A (en) * | 2013-12-13 | 2014-03-19 | 南京理工大学 | 2,3-Dihydroxymethyl-2,3-dinitro-1,4-butanediol tetraacetate and synthetic method thereof |
| CN103724208A (en) * | 2013-12-13 | 2014-04-16 | 南京理工大学 | 2,3-dihydromethyl-2,3-binitro-1,4-butanediol tetrapropionate and synthesis method thereof |
| CN105801323A (en) * | 2016-03-25 | 2016-07-27 | 徐志祥 | Preparing method for phase-stable ammonium nitrate |
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| NL67443C (en) * | 1947-09-01 | |||
| CA2464278A1 (en) * | 2004-04-08 | 2005-10-08 | Christopher Preston | Ammonium nitrate blasting agent and method of production |
| CN1274643C (en) * | 2004-08-11 | 2006-09-13 | 殷海权 | Crystal shape modifier for anmonium nitrate |
| JP5353000B2 (en) * | 2007-05-29 | 2013-11-27 | 東洋インキＳｃホールディングス株式会社 | Method for producing polyester resin and pressure-sensitive adhesive composition |
| CN100572343C (en) * | 2007-08-29 | 2009-12-23 | 黄东平 | Ammonium nitrate modifier and preparation method thereof |
| CN103012194B (en) * | 2012-11-16 | 2014-09-17 | 南京理工大学 | Nitrine ester compound and synthesis method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103641670A (en) * | 2013-12-13 | 2014-03-19 | 南京理工大学 | Method for coating RDX cyclotrimethylene trinitramine and HMX cyclotetramethylene tetranitramine and coating material thereof |
| CN103641723A (en) * | 2013-12-13 | 2014-03-19 | 南京理工大学 | 2,3-Dihydroxymethyl-2,3-dinitro-1,4-butanediol tetraacetate and synthetic method thereof |
| CN103724208A (en) * | 2013-12-13 | 2014-04-16 | 南京理工大学 | 2,3-dihydromethyl-2,3-binitro-1,4-butanediol tetrapropionate and synthesis method thereof |
| CN103641670B (en) * | 2013-12-13 | 2016-04-20 | 南京理工大学 | A kind of method of coating RDX and HMX and coating material thereof |
| CN105801323A (en) * | 2016-03-25 | 2016-07-27 | 徐志祥 | Preparing method for phase-stable ammonium nitrate |
| CN105801323B (en) * | 2016-03-25 | 2018-06-26 | 内蒙聚力工程爆破有限公司 | A kind of preparation method of phase stable ammonium nitrate |
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Application publication date: 20130626 |