CN100378041C - High temperature-resisting detonating fuse technology at 180 degrees C and for 48 hours - Google Patents
High temperature-resisting detonating fuse technology at 180 degrees C and for 48 hours Download PDFInfo
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- CN100378041C CN100378041C CNB2005100664380A CN200510066438A CN100378041C CN 100378041 C CN100378041 C CN 100378041C CN B2005100664380 A CNB2005100664380 A CN B2005100664380A CN 200510066438 A CN200510066438 A CN 200510066438A CN 100378041 C CN100378041 C CN 100378041C
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Abstract
The present invention relates to a 180 DEG C/48 hours high temperature resisting detonating fuse which is composed of new explosive and new materials and a fuse manufacturing technology thereof. The fuse manufacturing technology adopts HMX: KP=90: 10 and is added with 3 percent of fluororubber and 0.5 percent of graphite; potassium picrate with regular crystal form and uniform granularity is made by the control technology of optimizing crystal form; the preparation and the granulation of high temperature resisting explosive are completed by the technology of a suspension method. High temperature resisting materials, such as terylene PTE, polyester film BOPET, fluoroplastics, etc., are used for manufacturing the 180 DEG C/48 hours high temperature resisting detonating fuse by improving the condition of fuse manufacture. The explosive charging quantity of the detonating fuse is larger than 18 g/m; the external diameter is 5.3mm, detonating velocity is larger than 6800 m/s, temperature resistance is 180 DEG C/48 hours, voltage resistance is more than 60MPa, the detonating fuse can be reliably detonated by a No. 8 detonator, and a petroleum perforating bullet can be reliably detonated. The technology is mainly used for the exploitation of deep-layer oil and gas wells in civil detonating industry and can be also used for the detonation of deep water, or high temperature and high pressure work environments.
Description
Technical field
The present invention utilizes the solution water suspension method that the heatproof energetic material is carried out formulating of recipe and preparation, makes the industrial detonating fuse of high temperature resistant 180 ℃/48h; Be mainly used in the exploitation of the quick-fried industry mid-deep strata of people oil, gas well.
Background technology
In recent years, along with the raising of the total journey state of the art of oil and gas well drilling, oil and gas exploitation extends to the 5000m degree of depth from 3000m to the development of depths, stratum.Well depth increases, the ground environment temperature raises, and it is also more and more higher that oil gas well mining perforation equipment resistance toheat is required, and according to petroleum department's standard, the primacord fuse of anti-170 ℃/48h is called the ultrahigh-temperature primacord fuse.Primacord fuse is as one of series product of perforation equipment, and is more and more higher to its security and reliability requirement, and the performance of the high temperature powder of filling directly determines the security and the reliability of primacord fuse.
The high temperature powder commonly used of report has diamino hexanitrodiphenyl (DIPAM), octogen (HMX), hexanitro-stilbene (HNS), Ta Kete (TACOT), nine nitrotrimethylolmethane biphenyl (NONA), skin Weeks (PYX), eight nitrotrimethylolmethane biphenyl (ONT), triamino trinitrobenzene (TATB) and diamino trinitrobenzene (DATB) etc. both at home and abroad at present.Wherein, TATB, DIPAM, HNS and TACOT are the high temperature powders of external primary study, production and use.Consider from safety in production and application point of view, these explosives can not directly be loaded in the primacord fuse, after they need and mix through recipe configuration, form even particle distribution, free-running property good, to machinery and static insensitiveness, confection that explosion transfer performance is good, just can make primacord fuse then.
At present, the kind of domestic and international high temperature resistant primacord fuse is few, and main products is shown in Table 1.
Table 1 is high temperature resistant primacord fuse title and performance
| Title | Country origin | Powder charge | Heat-resisting | Remarks |
| HMX HNS HNS PYX60-130 RDX NRL-1 PF-S1 80RDX 80HMX 80PYX | In in in in the Mei Meimei U.S.-China | HMX HNS-I HNS-II PYX 1871 HFSIC PYX RDX HMX PYX | 200 ℃/200h of 250 ℃/24h of 190 ℃/200h of 260 ℃/1h of 146 ℃/200h, 177 ℃/24h of 150 ℃/24h of 230 ℃/48h of 180 ℃ of 220 ℃/2h | Grand celebration perforating bullet factory of relevant Beijing Institute of Technology with material.。。。。。 |
HMX can change brilliant at 167 ℃～183 ℃ in the table, transfers the δ type to by the β type, has unstable, has influenced its application to a certain extent; And the production cost height of explosives such as HNS, PYX, price is also more expensive, at the heavy duty service that is used for 6000～7000m aspect the petroleum perforation equipment more.Therefore, developing a kind of novel, with low cost, high temperature resistant primacord fuse of being adapted at the 5000m deep mining, is pressing for of market.
From the result for retrieval analysis, the maximum load that the heat-resisting primacord fuse of present domestic patent report can bear is 170 ℃, 80MPa, and this is the patent that we applied in 1987.Remove in addition, do not see the production line that the high temperature and high load lotus primacord fuse of anti-180 ℃/48h is arranged and the report of corresponding technology.Foreign patent has the production technique of heat-resisting primacord fuse, but its performance index are not appeared in the newspapers.
Summary of the invention
This invention is to the effect that: the powder charge formulating of recipe of (1) 180 ℃/48h ultrahigh-temperature primacord fuse.Comprise main body explosive, tackiness agent, deterrent formulating of recipe and preparation technology.(2) high temperature resistant primacord fuse structure design and technical study.(3) high temperature resistant primacord fuse performance test.
1.180 ℃/the powder charge prescription of 48h ultrahigh-temperature primacord fuse
The main body explosive that the present invention selects for use is HMX.The price of this explosive is the most cheap a kind of in the listed explosive of table 1, and its fusing point is 276 ℃, but 195 ℃ of 2 hours heatproofs heat 48 hours continuously, but 165 ℃ of heatproofs.This index can't satisfy the requirement of 180 ℃/48h, and in order to improve the thermotolerance of HMX, the present invention selects for use low price, dystectic priming charge potassium picrate (KP) as auxiliary powder charge.The decomposition peak of potassium picrate is 358.85 ℃ of (20 ℃ of min
-1), the 5s bursting point is 391 ℃, impact sensitivity, friction sensitivity are equivalent to high explosive, to static very insensitiveness.100 ℃ of vacuum stability discharge quantities are 0.21mlg
-1, 100 ℃/48h thermal weight loss has only 0.13%.
Except that explosive, tackiness agent is selected viton for use, is characterized in having good storage stability, electrical insulating property and radioresistance; Good oil resistant, resistance to medium; Good heat resistance usually can be at 250 ℃ of following life-time service.Deterrent adopts graphite material, and it has good lubrication; Fusing point is more than 3000 ℃; Specific heat is bigger, is 7kJ/kg, and thermal conductivity is less, is 50.24W/mK.
The proportioning of above-mentioned confection is HMX: KP=80: 20, add 3% viton and 0.5% graphite in addition.
2. potassium picrate is optimized crystalline form preparation technology
Picric acid solution is obtained sodium picrate with yellow soda ash neutralization, carry out recrystallization with the sodium picrate of concentrated nitric acid and generation again and can generate little acicular picric acid.Reaction principle is as follows:
(1) neutralization reaction
(2) recrystallization
Picric acid and 20ml crystal control agent with 10.0g after refining are put into beaker, add a small amount of distilled water, as end liquid, this mixing solutions is put into water bath with thermostatic control, bath temperature is 35 ℃, stirring velocity is 300rpm, drip potassium hydroxide solution 100ml, according to the different purposes control dropping times, dropwise and continue to stir and insulation 10min, reduce to discharging after the room temperature, respectively once with distilled water, each washing of dehydrated alcohol, carry out suction filtration with B, place baking oven dry 6h under 60 ℃ then.
The potassium picrate crystalline form rule, the size ratio that adopt optimization crystalline form control techniques to prepare are more even.
3. water suspension method technology is made up a prescription
HMX and KP are placed beaker according to 8: 2 common 19.4g of proportioning, add water 200g, dispersant solution 1.5～3.0m1 and defoamer solution 1.0～1.2ml simultaneously.Reinforced finishing put into water bath with thermostatic control with beaker, and the control bath temperature is at 30 ℃, and the solution that stirs the mixture is until forming homodisperse suspension.Then bath temperature is warmed up to 85 ± 2 ℃ with the speed of about 3 ℃/min, under violent stirring, 60ml is added drop-wise in the suspension with viton solution.After feed liquid added, constant temperature stirred 2～3 minutes, added water 30ml.Discharging after 5 minutes adds a large amount of cold water washings, suction filtration, and oven dry promptly obtains the particulate state high temperature powder.
4. high temperature resistant primacord fuse structure
The high temperature resistant primacord fuse of 180 ℃/48h is made up of high temperature powder, heart yearn, medicine film, interior layer line, zero line, outer layer line and coating.Its materials used and size see Table 2.
Table 2 is high temperature resistant primacord fuse material and size
| Heart yearn | The medicine film | Interior layer line | Middle level, outer layer line | The outer coating | |
| Material | The PET staple | The PET polyester | The PET silk | The PET silk | Fluoroplastics |
| Size | 3 strands | 25×0.03mm | 13 | 10 | Φ5.3mm |
Description of drawings
180 ℃/48h of Fig. 1 is high temperature resistant primacord fuse structural representation;
Among the figure: 1. coating, 2. outer layer line, 3. zero line, 4. in layer line, 5. medicine film, 6. high temperature resistant explosive, 7. heart yearn.
Column potassium picrate crystalline form before Fig. 2 a optimal control
Particulate state potassium picrate crystalline form after Fig. 2 b optimal control
Particulate state potassium picrate crystalline form after Fig. 2 c optimal control
The high temperature resistant medicament of 180 ℃/48h of Fig. 3 is heated and is tested the sample of front and back
180 ℃/48h of Fig. 4 is high temperature resistant primacord fuse sample
180 ℃/48h of Fig. 5 is high temperature resistant primacord fuse production scheme
Embodiment
Potassium picrate prepares embodiment:
(1) batching 5% crystal control agent, 15% potassium hydroxide solution.
(2) in and picric acid: yellow soda ash=1: 0.42 (picric acid feed intake 2kg), in beaker, add load weighted picric acid and distilled water, this beaker is put into 85 ℃ of waters bath with thermostatic control heat.Heated while stirring stirring velocity 500Rpm 15 minutes.Add yellow soda ash then, up to reacting completely.
(3) recrystallization filters above-mentioned sodium salt solution, removes impurity.The filtrate low whipping speed is under the 50Rpm, slowly adds the nitric acid of concentration 66～68%, till no flocculent precipitate is separated out.
(4) suction filtration is with recrystallized product suction filtration on suction filter.Must make with extra care little needle-like picric acid wet feed.
(5) dry with the picric acid wet feed drying after the exquisiteness.60 ℃ of bake out temperatures, 6 hours time.
(6) the refining picric acid of chemical combination: potassium hydroxide: crystal control agent=1: 0.25: 0.05, in 61 combination apparatus, add load weighted refining picric acid, distilled water and crystal control agent liquid 500ml, heat while stirring, make the picric acid wet feed be suspension, churning time 15min, stirring velocity 500Rpm.
Drip potassium hydroxide solution 2000ml, at the uniform velocity reinforced, feed rate is controlled by volume pump, and reinforced time 15～20min after feed liquid adds, continues to stir 5～10min, gets yellow or tawny granule crystal.
(7) take out and wash bonded potassium picrate solution with distilled water washing 5 times.Embathe 2 times with alcohol.
(8) suction filtration is with above-mentioned product suction filtration on suction filter.During suction filtration, available dehydration of alcohol.Carry out the branch dish behind the suction filtration.
(9) dry with potassium picrate wet feed drying.60 ℃ of drying temperatures, 6 hours time.
25 ℃ of relative humidity of stock's temperature are not more than 65%.
Water suspension method pharmacy embodiment:
(1) the viton solution of preparation 3% concentration
Ethyl acetate adding volume is counted V and is calculated as follows:
0.9-the proportion of ethyl acetate, the concentration of solution that 0.01-joins, the volume number that the V-ethyl acetate adds, the quality that the G-viton adds.
Measure ethyl acetate to going in the bottle, viton is cut into small pieces again, accurately weighing is poured in the same port grinding bottle, and every 2h stirs once, stirs overnight can the use altogether 3 times.
(2) HMX and KP were according to 8: 2 proportionings, and the viton solution that adds 3% concentration carries out granulation.
With 2.0kg confection and 2500ml concentration is the aqueous dispersant of 0.25g/l, places tablets press, begins to stir, and makes confection suspended dispersed in aqueous dispersant even.Feeding hot water in chuck makes aqeous suspension be warmed up to 65～70 ℃.Open vacuum system, vacuum tightness is about 15.0KPa in making, and opens the water of condensation valve, adds the viton solution that has prepared by the tablets press upper pipe, and suitably regulator solution adds speed so that control size.Be incubated about 10～20min again after adding solution, be warmed up to 70～75 ℃ then, vacuum tightness is raised to about 30KPa, to steam residual solvent.Feed cold water to chuck and make the material cooling, when material is cooled to below 40 ℃, open tablets press bottom valve blowing.
(3) filter, wash and drying.Above-mentioned material is put in the rinse bath, and suction filtration removes the granulation mother liquor, washes the particle three times on the strainer with water, and the about 20min of suction at last is placed on particle then in the loft drier that the aluminium dish is built in 80 ℃ and dries 8～10h.
(4) insensitiveness is handled.In drum,, under 60～80r/min, mix 8～10min and get final product by the load weighted graphite of 0.5% adding.
High temperature resistant primacord fuse is made embodiment:
180 ℃/48h is high temperature resistant, and the primacord fuse Production Flow Chart is as follows: (see figure 5)
(1) refining potassium picrate is dried the HMX after sieving.
(2) make high temperature resistant explosive with the suspension comminution granulation.
(3) mix medicine method passivation high temperature powder with machinery, and oven dry.
(4) heart yearn is fixed on the drum of upper end, internal coating is placed on drum position, upper strata.
(5) middle level and the outer bobbin that coats are placed on respectively on two roads, three roads and the extreme trace drum.
(6) good medicine mouth of Installation and Debugging and snap gauge.
(7) start system rope.
(8) the primacord fuse coating plastic behind the fake.
(9) fake, drying and vanning.
(10) stamped mark
(12) performance test, check, packing and warehouse-in.
Claims (3)
1. primacord fuse, this primacord fuse comprises: 1. main blasting charge is characterized in that explosive is made up of HMX, KP, viton and graphite; 2. coating material is characterized in that coating layer is made up of PTE silk, BOPET film.
2. primacord fuse as claimed in claim 1, its main blasting charge adopts HMX: KP=80: 20, add 3% viton and 0.5% graphite in addition.
3. primacord fuse as claimed in claim 1, its coating material comprises: terylene PTE staple and biaxially oriented polyester film BOPET.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100664380A CN100378041C (en) | 2005-04-25 | 2005-04-25 | High temperature-resisting detonating fuse technology at 180 degrees C and for 48 hours |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100664380A CN100378041C (en) | 2005-04-25 | 2005-04-25 | High temperature-resisting detonating fuse technology at 180 degrees C and for 48 hours |
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| Publication Number | Publication Date |
|---|---|
| CN1854112A CN1854112A (en) | 2006-11-01 |
| CN100378041C true CN100378041C (en) | 2008-04-02 |
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| CNB2005100664380A Expired - Fee Related CN100378041C (en) | 2005-04-25 | 2005-04-25 | High temperature-resisting detonating fuse technology at 180 degrees C and for 48 hours |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103145512B (en) * | 2013-03-13 | 2014-12-10 | 中国工程物理研究院化工材料研究所 | High-gurney-energy low-vulnerability PBX explosive and preparation method thereof |
| CN103772079A (en) * | 2014-01-13 | 2014-05-07 | 云南燃二化工有限公司 | Permissible detonating cord for coal mine, and cord maker thereof |
| CN108892596A (en) * | 2018-07-23 | 2018-11-27 | 江西赣州国泰特种化工有限责任公司 | A kind of medicine core and preparation method thereof of water resistant primacord |
| CN109988069A (en) * | 2018-08-31 | 2019-07-09 | 山西壶化集团股份有限公司 | A kind of preparation method of potassium picrate |
| CN111138237A (en) * | 2020-01-19 | 2020-05-12 | 陕西渭南庆华化工有限公司 | Low-energy flexible detonating cord |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4316412A (en) * | 1979-06-05 | 1982-02-23 | The United States Of America As Represented By The United States Department Of Energy | Low voltage nonprimary explosive detonator |
| CN1033178A (en) * | 1987-11-19 | 1989-05-31 | 北京工业学院 | Heat-resistance high mixed explosive |
| WO2000026603A1 (en) * | 1998-11-04 | 2000-05-11 | Orica Explosives Technology Pty. Ltd. | Non-primary detonators |
-
2005
- 2005-04-25 CN CNB2005100664380A patent/CN100378041C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4316412A (en) * | 1979-06-05 | 1982-02-23 | The United States Of America As Represented By The United States Department Of Energy | Low voltage nonprimary explosive detonator |
| CN1033178A (en) * | 1987-11-19 | 1989-05-31 | 北京工业学院 | Heat-resistance high mixed explosive |
| WO2000026603A1 (en) * | 1998-11-04 | 2000-05-11 | Orica Explosives Technology Pty. Ltd. | Non-primary detonators |
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| CN1854112A (en) | 2006-11-01 |
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Effective date of registration: 20090925 Address after: 5, Zhongguancun South Street, Haidian District, Beijing, zip code: 100081 Co-patentee after: The Yunnan Refco Group Ltd. Patentee after: BEIJING INSTITUTE OF TECHNOLOGY Address before: 5, Zhongguancun South Street, Haidian District, Beijing, zip code: 100081 Co-patentee before: Yunnan Raner Chemical Industry Co., Ltd. Patentee before: BEIJING INSTITUTE OF TECHNOLOGY |
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Granted publication date: 20080402 Termination date: 20160425 |