CN104628496A - High-temperature-resistant propellant for oil/gas deep well and preparation method of high-temperature-resistant propellant - Google Patents
High-temperature-resistant propellant for oil/gas deep well and preparation method of high-temperature-resistant propellant Download PDFInfo
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- CN104628496A CN104628496A CN201510078336.4A CN201510078336A CN104628496A CN 104628496 A CN104628496 A CN 104628496A CN 201510078336 A CN201510078336 A CN 201510078336A CN 104628496 A CN104628496 A CN 104628496A
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Abstract
The invention provides a high-temperature-resistant propellant for an oil/gas deep well. The high-temperature-resistant propellant is prepared from the following raw materials by weight percent: 30 to 58 percent of potassium perchlorate, 2 to 30 percent of 1,1'-dihydroxyl-5,5'-bistetrazole dihydroxylamine salt, 10 to 20.90 percent of high-temperature-resistant epoxy resin, 0 to 16.58 percent of bisphenol A epoxy resin, 4.75 to 13.03 percent of epoxy resin active diluting agent, 0.5 percent of accelerant boron trifluoride-amine complex, 0.03 percent of a defoaming agent, 6.57 to 8.14 percent of diaminodiphenyl sulfone, and the sum of the weight percentage of the raw materials is 100 percent. The raw materials of the propellant are mixed after being pre-mixed, and then the mixed materials are formed by virtue of a mold to produce a finished product. After the solid propellant is immersed in clean water and 3.5% saline water for 24 to 48 hours, the weight loss of the solid propellant is less than 3 percent, and the volume variation is less than 2 percent; the temperature-resistant grade can reach 200 DEG C for 48 hours, the spontaneous combustion of the propellant can be avoided, and the high-temperature-resistant propellant can be used in a high-temperature watery environment.
Description
Technical field
The invention belongs to oil/gas deep well heat-resisting Pressure breaking bullet powder charge field, relate to a kind of propelling agent.
Background technology
Utilize the explosion fracturing of the powder charge at home and abroad developing history of existing nearly 40 years, box hat formula, is used widely in oil field without the multiple Pressure breaking bullet products such as shell-type or technology, achieves good increasing yield and injection effect.Explosion fracturing technology utilizes specific propellant charge in the pay sand high velocity combustion of Oil/gas Well, produce High Temperature High Pressure pulse gas, fracturing stratum forms many from the radial radial fissure of well, remove hydrocarbon contamination and tamper, effectively reduce stratum skin factor, thus reach the object of well production increment.
During due to oil well operation, the subsurface environment residing for Pressure breaking bullet is many water surroundings of high temperature (200 DEG C), and common HTPB propellant heat resistance is poor, and heatproof is at 150 DEG C; And HTPB propellant contains a large amount of ammoniumper chlorate, the solubleness of ammoniumper chlorate in water is larger.Therefore, such propelling agent cannot meet the demands.
Chinese patent (publication number CN 1275556A) " the hot hole composition of high temperature resistant solid propellant and synergistic perforator " discloses a kind of high temperature resistant solid propellant, comprises 45 ~ 60% oxygenants, 35 ~ 50% reductive agents and 2 ~ 15% sensitizing agents.In this is high temperature resistant solid propellant, oxygenant is the oxysalt (as saltpetre) of inorganic high-temperature resistant, reductive agent is resistant to elevated temperatures organic polymer material (as polyurethane elastomer, rubber, high-temperature adhesives etc.), sensitizing agent is metal-powder, can be the metal-powder that magnesium powder or aluminium powder or aluminum magnesium alloy etc. are more active, granularity 50 ~ 200 order.Saltpetre solubleness in water is comparatively large, and 20 DEG C of solubleness are 31.6 grams, and 50 DEG C of solubleness are 85.5 grams, and temperature more high-dissolvability is larger, therefore can not to use in many water surroundings of high temperature (being greater than 150 DEG C).
Summary of the invention
For the deficiencies in the prior art, the object of the invention is to, the high temperature resistant solid propellant of oil/gas deep well that a kind of explosion fracturing bullet powder charge field being applicable to oil field deep well can use in the many water surroundings of high temperature is provided.
In order to realize above-mentioned task, the present invention adopts following technical scheme to be achieved:
The high temperature resistant solid propellant of a kind of oil/gas deep well, by weight percentage: potassium perchlorate is 30% ~ 58%, 1,1 '-dihydroxyl-5,5 '-bistetrazole dihydroxy amine salt is 2% ~ 30%, high-temperature-resistant epoxy resin is 10% ~ 20.9%, bisphenol A epoxide resin is 0 ~ 16.58%, epoxide resin reactive diluent is 4.75 ~ 13.03%, promotor boron trifluoride-amine complex is 0.5%, and defoamer is 0.03%, and diaminodiphenylsulfone(DDS) is 6.57% ~ 8.14%, raw material weight percentage ratio summation is 100%, wherein:
Described bisphenol A epoxide resin is epoxy resin E-51;
Described high-temperature-resistant epoxy resin is 4,4 '-diaminodiphenylmethane four glycidyl amine type epoxy resin, 3,4 '-diaminodiphenyl oxide four glycidyl amine type epoxy resin or 4,4 '-diaminodiphenyl oxide four glycidyl amine type epoxy resin;
Described epoxide resin reactive diluent is o-tolyl glycidyl ether or polyethyleneglycol diglycidylether;
Described defoamer is silicone resin.
The high temperature resistant solid propellant of preferred oil/gas deep well, by weight percentage: potassium perchlorate is 30%, 1,1 '-dihydroxyl-5,5 '-bistetrazole dihydroxy amine salt is 30%, 4,4 '-diaminodiphenylmethane four glycidyl amine type epoxy resin is 14.4%, and epoxy resin E-51 is 5.47%, o-tolyl glycidyl ether is 13.03%, promotor 0.5%, silicone resin is 0.03%, and diaminodiphenylsulfone(DDS) is 6.57%.
The above-mentioned oil/gas deep well preparation method of high temperature resistant solid propellant, the method is carried out according to following steps:
Step one, according to formula rate, by high-temperature-resistant epoxy resin, bisphenol A epoxide resin, epoxide resin reactive diluent for, promotor boron trifluoride-amine complex, defoamer add in mixing kettle, premix 10 minutes;
Step 2, by weight percentage, adds potassium perchlorate, 1 in the system of step one, after 1 '-dihydroxyl-5,5 '-bistetrazole dihydroxy amine salt mixes 50 minutes, then adds diaminodiphenylsulfone(DDS), mixes after 15 minutes and stops mixing, obtains medicine slurry;
Step 3, by medicine slurry be poured in mould, put into 130 DEG C oven for curing, 72 hours, move back mould, obtain high temperature resistant solid propellant finished product.
Compared with prior art, useful technique effect is in the present invention:
(1) solid propellant excellent hydrolysis resistance of the present invention, the medicine block of 50mm × 50mm × 20mm soaks and reaches 24 ~ 48 hours in clear water and 3.5% salt solution, and weightlessness is less than 3%, and volume change is less than 2%, considerable change does not occur.And the poor-performing of the resistance to tap water of existing solid propellant and 3.5% salt solution.
(2) heat resistance of the present invention is better, heatproof rank reach 200 DEG C 48 hours, there is not spontaneous combustion, can use in the many water surroundings of high temperature.
Embodiment
Defer to technique scheme, following embodiment provides the high temperature resistant solid propellant of a kind of oil/gas deep well, by weight percentage: potassium perchlorate is 30% ~ 58%, 1, 1 '-dihydroxyl-5, 5 '-bistetrazole dihydroxy amine salt is 2.00% ~ 30%, high-temperature-resistant epoxy resin is 10% ~ 20.9%, bisphenol A epoxide resin is 0 ~ 16.58%, epoxide resin reactive diluent is 4.75 ~ 13.03%, promotor boron trifluoride-amine complex is 0.5%, defoamer is 0.03%, diaminodiphenylsulfone(DDS) is 6.57% ~ 8.14%, raw material weight percentage ratio summation is 100%, wherein:
Described bisphenol A epoxide resin is epoxy resin E-51;
Described high-temperature-resistant epoxy resin is 4,4 '-diaminodiphenylmethane four glycidyl amine type epoxy resin, 3,4 '-diaminodiphenyl oxide four glycidyl amine type epoxy resin or 4,4 '-diaminodiphenyl oxide four glycidyl amine type epoxy resin;
Described epoxide resin reactive diluent is o-tolyl glycidyl ether or polyethyleneglycol diglycidylether;
Described defoamer is silicone resin.
The high temperature resistant solid propellant of preferred oil/gas deep well, by weight percentage, is made up of following raw material: potassium perchlorate is 30%, 1,1 '-dihydroxyl-5,5 '-bistetrazole dihydroxy amine salt is 30%, 4,4 '-diaminodiphenylmethane four glycidyl amine type epoxy resin is 14.4%, epoxy resin E-51 is 5.47%, and o-tolyl glycidyl ether is 13.03%, promotor 0.5%, silicone resin is 0.03%, and diaminodiphenylsulfone(DDS) is 6.57%.
The specification requirement of above-mentioned raw materials is as follows:
1,1 '-dihydroxyl-5,5 '-bistetrazole dihydroxy amine salt is industrial goods, yellow solid powder, granularity (< 1.5 μm)>=92%, density 1.938g/cm
3, acid number (PH) 4 ~ 7.Can from buyings such as triumphant examination (Shanghai) Science and Technology Ltd., Shanghai Tao Suo biochemical technology company limited and spring westernization factories of Huixian City of Henan Province.1, the structural formula of 1 '-dihydroxyl-5,5 '-bistetrazole dihydroxy amine salt (HATO) is as follows:
4,4 '-diaminodiphenylmethane four glycidyl amine type epoxy resin (being abbreviated as TGDDM), reddish-brown is amber thick liquid extremely, oxirane value >=0.8 equivalent/100g, viscosity 3.0 ~ 7.0Pas (50 DEG C).The structural formula of TGDDM is as follows:
The oxirane value of epoxy resin E-51 is 0.48 ~ 0.54, and viscosity 6.0 ~ 10.0Pas (25 DEG C), polymerization degree n=0.1 ~ 0.28, relative molecular mass is 307 ~ 420.The molecular formula of epoxy resin E-51 is as follows:
O-tolyl glycidyl ether outward appearance is colourless to light yellow transparent liquid, and oxirane value is 0.50 ~ 0.54 equivalent/100g, and 25 DEG C of viscositys are 5 ~ 10mPas.
Polyethyleneglycol diglycidylether outward appearance is colourless to light yellow transparent liquid, and oxirane value is 0.30 ~ 0.36 equivalent/100g, and 25 DEG C of viscositys are 50 ~ 70mPas.
The viscosity of silicone resin is (100 ~ 1100) × 10
-6m
2/ s, refractive index n
d 251.400 ~ 1.410.
The above-mentioned oil/gas deep well preparation method of high temperature resistant solid propellant, the method is carried out according to following steps:
Step one, according to formula rate, by weight percentage, be 10.00% ~ 20.90% by high-temperature-resistant epoxy resin, bisphenol A epoxide resin is 0 ~ 16.58%, and epoxide resin reactive diluent is 4.75 ~ 13.03%, promotor boron trifluoride-amine complex is 0.50%, defoamer is 0.03%, adds in mixing kettle, premix 10 minutes;
Step 2, by weight percentage, in the system of step one, add potassium perchlorate is 30.00% ~ 58.00%, 1,1 '-dihydroxyl-5,5 '-bistetrazole dihydroxy amine salt is 2.00% ~ 30.00%, mix after 50 minutes, adding diaminodiphenylsulfone(DDS) is again 6.57% ~ 8.14%, mixes after 15 minutes and stops mixing, obtains medicine slurry;
Step 3, the medicine that step 2 is obtained slurry be poured in mould, put into 130 DEG C oven for curing, 72 hours, move back mould, obtain high temperature resistant solid propellant finished product.
Below provide specific embodiments of the invention, it should be noted that the present invention is not limited to following specific embodiment, all equivalents done on technical scheme basis all fall into protection scope of the present invention.
Embodiment 1:
The high temperature resistant solid propellant of oil/gas deep well of the present embodiment, by weight percentage, be made up of following raw material: potassium perchlorate is 30.00%, 1,1 '-dihydroxyl-5,5 '-bistetrazole dihydroxy amine salt is 30.00%, 4,4 '-diaminodiphenylmethane four glycidyl amine type epoxy resin is 14.40%, epoxy resin E-51 is 5.47%, and o-tolyl glycidyl ether is 13.03%, and promotor boron trifluoride-amine complex is 0.50%, silicone resin is 0.03%, and diaminodiphenylsulfone(DDS) is 6.57%.
Performance test:
Quick-fried heat presses the quick-fried heat of GJB770B-2005 method 701.2 and combustion heat constant temperature method measures.
Specific volume is pressed GJB770B-2005 method 702.1 specific volume pressure transmitter method and is measured.
High thermal resistance testing method is: Ф 20mm × 20mm powder column (1) 3 DEG C/min rises to 200 DEG C, insulation 48h; (2) temperature controlling point: thermopair is suspended from directly over sample, not with sample contacts.Sample thermal weight loss is not more than 3%, does not fire not quick-fried being by test.
Propelling agent is water-fast, and testing method is: 50mm × 50mm × 20mm medicine block submergence 48h in tap water, and weightlessness is less than 3%, and volume change is less than 2%, is by test.
The oil/gas deep well of the present embodiment by the properties test result of high temperature resistant solid propellant in table 1.
Table 1 embodiment 1 properties test result
As can be drawn from Table 1, the quick-fried heat (i.e. energy) of this propelling agent is slightly high, and specific volume is moderate, and resistance to elevated temperatures, water resistance and salt water resistance performance all reach performance requriements.Be applicable to the heat-resisting Pressure breaking bullet powder charge of oil/gas deep well to use.
Embodiment 2:
The high temperature resistant solid propellant of oil/gas deep well of the present embodiment, by weight percentage, be made up of following raw material: potassium perchlorate is 35.00%, HATO is 25.00%, TGDDM is 10.00%, and epoxy resin E-51 is 16.58%, o-tolyl glycidyl ether is 4.75%, promotor boron trifluoride-amine complex is 0.50%, and silicone resin is 0.03%, and diaminodiphenylsulfone(DDS) is 8.14%.
The oil/gas deep well of the present embodiment is identical with embodiment 1 with the performance test methods of high temperature resistant solid propellant, and properties test result is in table 2.
Table 2 embodiment 2 properties test result
As can be drawn from Table 2, the quick-fried heat (i.e. energy) of this propelling agent is moderate, and specific volume is moderate, and resistance to elevated temperatures, water resistance and salt water resistance performance all reach performance requriements.Be applicable to the heat-resisting Pressure breaking bullet powder charge of oil/gas deep well to use.
Embodiment 3:
The high temperature resistant solid propellant of oil/gas deep well of the present embodiment, by weight percentage, be made up of following raw material: potassium perchlorate is 58.00%, HATO is 2.00%, TGDDM is 20.90%, and o-tolyl glycidyl ether is 11.25%, and promotor boron trifluoride-amine complex is 0.50%, silicone resin is 0.03%, and diaminodiphenylsulfone(DDS) is 7.32%.
The oil/gas deep well of the present embodiment is identical with embodiment 1 with the performance test methods of high temperature resistant solid propellant, and properties test result is in table 3.
Table 3 embodiment 3 properties test result
As can be drawn from Table 3, the quick-fried heat (i.e. energy) of this propelling agent is moderate, and specific volume is moderate, and resistance to elevated temperatures, water resistance and salt water resistance performance all reach performance requriements.Also be applicable to the heat-resisting Pressure breaking bullet powder charge of oil/gas deep well to use.
Above in all embodiments, raw material o-tolyl glycidyl ether can be replaced with polyethyleneglycol diglycidylether, raw material 4,4 '-diaminodiphenylmethane four glycidyl amine type epoxy resin (being abbreviated as TGDDM) can with 3,4 '-diaminodiphenyl oxide four glycidyl amine type epoxy resin (is abbreviated as 3,4 '-TGDDE) or 4,4 '-diaminodiphenyl oxide four glycidyl amine type epoxy resin (is abbreviated as 4,4 '-TGDDE) replace, technique effect is identical, in view of length, corresponding embodiment will be provided no longer one by one.
Claims (3)
1. the high temperature resistant propelling agent of oil/gas deep well, it is characterized in that, by weight percentage, be made up of following raw material: potassium perchlorate is 30.00% ~ 58.00%, 1,1 '-dihydroxyl-5,5 '-bistetrazole dihydroxy amine salt is 2.00% ~ 30.00%, and high-temperature-resistant epoxy resin is 10.00% ~ 20.90%, and bisphenol A epoxide resin is 0 ~ 16.58%, epoxide resin reactive diluent is 4.75 ~ 13.03%, promotor is 0.50%, and defoamer is 0.03%, and diaminodiphenylsulfone(DDS) is 6.57% ~ 8.14%, raw material weight percentage ratio summation is 100%, wherein:
Described bisphenol A epoxide resin is epoxy resin E-51;
Described high-temperature-resistant epoxy resin is 4,4 '-diaminodiphenylmethane four glycidyl amine type epoxy resin, 3,4 '-diaminodiphenyl oxide four glycidyl amine type epoxy resin or 4,4 '-diaminodiphenyl oxide four glycidyl amine type epoxy resin;
Described epoxide resin reactive diluent is o-tolyl glycidyl ether or polyethyleneglycol diglycidylether;
Described defoamer is silicone resin;
Described promotor is boron trifluoride-amine complex.
2. the high temperature resistant solid propellant of oil/gas deep well as claimed in claim 1, it is characterized in that, by weight percentage, be made up of following raw material: potassium perchlorate is 30.00%, 1,1 '-dihydroxyl-5,5 '-bistetrazole dihydroxy amine salt is 30.00%, 4,4 '-diaminodiphenylmethane four glycidyl amine type epoxy resin is 14.40%, and epoxy resin E-51 is 5.47%, o-tolyl glycidyl ether is 13.03%, promotor 0.50%, silicone resin is 0.03%, and diaminodiphenylsulfone(DDS) is 6.57%.
3. the oil/gas deep well preparation method of high temperature resistant solid propellant as claimed in claim 1, it is characterized in that, the method is carried out according to following steps:
Step one, according to formula rate, adds in mixing kettle by high-temperature-resistant epoxy resin, bisphenol A epoxide resin, epoxide resin reactive diluent, boron trifluoride-amine complex, defoamer, premix 10 minutes;
Step 2, adds potassium perchlorate, 1 in mixing kettle, 1 '-dihydroxyl-5,5 '-bistetrazole dihydroxy amine salt, mixes after 50 minutes, then adds diaminodiphenylsulfone(DDS), mixes after 15 minutes and stops mixing, obtains medicine slurry;
Step 3, by medicine slurry be poured in mould, put into 130 DEG C oven for curing, 72 hours, move back mould, obtain high temperature resistant solid propellant finished product.
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Citations (2)
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| CN103045143A (en) * | 2012-11-14 | 2013-04-17 | 浙江华正新材料股份有限公司 | Halogen-free epoxy adhesive and cover film prepared by using halogen-free epoxy adhesive |
| CN103304351A (en) * | 2013-05-29 | 2013-09-18 | 西安近代化学研究所 | High-temperature-resistant solid propellant for deep oil-gas well and preparation method thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103045143A (en) * | 2012-11-14 | 2013-04-17 | 浙江华正新材料股份有限公司 | Halogen-free epoxy adhesive and cover film prepared by using halogen-free epoxy adhesive |
| CN103304351A (en) * | 2013-05-29 | 2013-09-18 | 西安近代化学研究所 | High-temperature-resistant solid propellant for deep oil-gas well and preparation method thereof |
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| 余逸等: "防止液态2-乙基-4-甲基咪唑结晶的方法", 《热固性树脂》 * |
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