CN104628496B - A kind of oil/gas deep well high temperature resistant propellant and preparation method thereof - Google Patents
A kind of oil/gas deep well high temperature resistant propellant and preparation method thereof Download PDFInfo
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- CN104628496B CN104628496B CN201510078336.4A CN201510078336A CN104628496B CN 104628496 B CN104628496 B CN 104628496B CN 201510078336 A CN201510078336 A CN 201510078336A CN 104628496 B CN104628496 B CN 104628496B
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Abstract
The invention provides a kind of oil/gas deep well high temperature resistant propellant, by weight percentage：Potassium hyperchlorate is 30%~58%, 1, the bistetrazole dihydroxy amine salt of 1 ' dihydroxy 5,5 ' is 2%~30%, and high-temperature-resistant epoxy resin is 10%~20.90%, bisphenol A epoxide resin is 0~16.58%, epoxide resin reactive diluent is 4.75~13.03%, and accelerator boron trifluoride amine complex is 0.5%, and defoamer is 0.03%, diaminodiphenylsulfone is 6.57%~8.14%, and raw material weight percentage summation is 100%；The raw material of the propellant is remixed after premix, last mould molding, and finished product is made.The solid propellant was soaked in clear water and 3.5% salt solution up to 24~48 hours, and weightlessness is less than 3%, and Volume Changes are less than 2%；Heatproof rank reaches 200 DEG C 48 hours, does not occur spontaneous combustion, can be used in many water environments of high temperature.
Description
Technical field
The invention belongs to the heat-resisting Pressure breaking bullet powder charge field of oil/gas deep well, it is related to a kind of propellant.
Background technology
Using the explosion fracturing at home and abroad developing history of existing nearly 40 years of powder charge, box hat formula, without shell-type etc.
A variety of Pressure breaking bullet products or technology are used widely in oil field, achieve preferable increasing yield and injection effect.Explosion fracturing technology
It is the oil-producing formation high-velocity combustion using specific propellant loading in Oil/gas Well, produces HTHP pulse gas, fracturing stratum
Form a plurality of from the radial radial fissure of well, remove hydrocarbon contamination and tamper, be effectively reduced stratum epidermis system
Number, so as to reach the purpose of well production increment.
During due to oil well operation, the subsurface environment residing for Pressure breaking bullet is many water environments of high temperature (200 DEG C), and common fourth hydroxyl is pushed away
Enter agent heat resistance poor, heatproof is at 150 DEG C；And HTPB propellant contains substantial amounts of ammonium perchlorate, and ammonium perchlorate is in water
Solubility it is larger.Therefore, such propellant can not meet requirement.
Chinese patent (publication number CN 1275556A) " composition and synergistic perforating of high temperature well high temperature resistant solid propellant
Device " discloses a kind of high temperature resistant solid propellant, including 45~60% oxidants, 35~50% reducing agents and 2~15% are quick
Agent.Oxidant is the oxysalt (such as potassium nitrate) of inorganic high-temperature resistant in the high temperature resistant solid propellant, and reducing agent is resistance to height
The high-molecular organic material (such as polyurethane elastomer, rubber, high-temperature adhesives) of temperature, sensitizer is metal dust, Ke Yishi
The more active metal dust such as magnesium powder or aluminium powder or almag, the mesh of granularity 50~200.Potassium nitrate solubility in water is larger,
20 DEG C of solubility are 31.6 grams, and 50 DEG C of solubility are 85.5 grams, and temperature more high-dissolvability is bigger, therefore can not be (big in high temperature
In 150 DEG C) many water environments in use.
The content of the invention
For the deficiencies in the prior art, it is an object of the present invention to provide a kind of suitable for the quick-fried of oil field deep well
The oil/gas deep well high temperature resistant solid propellant that combustion Pressure breaking bullet powder charge field can be used in many water environments of high temperature.
In order to realize above-mentioned task, the present invention, which is adopted the following technical scheme that, to be achieved：
A kind of oil/gas deep well high temperature resistant solid propellant, by weight percentage：Potassium hyperchlorate is 30%~58%, 1,
1 '-dihydroxy -5,5 '-bistetrazole dihydroxy amine salt is 2%~30%, and high-temperature-resistant epoxy resin is 10%~20.9%, bisphenol-A ring
Oxygen tree fat is 0~16.58%, and epoxide resin reactive diluent is 4.75~13.03%, accelerator boron trifluoride-amine complex
For 0.5%, defoamer is 0.03%, and diaminodiphenylsulfone is 6.57%~8.14%, and raw material weight percentage summation is
100%, wherein：
Described bisphenol A epoxide resin is epoxy resin E-51；
Described high-temperature-resistant epoxy resin be the glycidyl amine type epoxy resin of 4,4 '-MDA four, 3,4 '-
The glycidyl amine type epoxy resin of diaminodiphenyl ether four or the glycidyl amine type epoxy resin of 4,4 '-diaminodiphenyl ether four；
Described epoxide resin reactive diluent is o-tolyl glycidol ether or polyethyleneglycol diglycidylether；
Described defoamer is silicone resin.
It is preferred that oil/gas deep well high temperature resistant solid propellant, by weight percentage：Potassium hyperchlorate is 30%, 1,1 '-
Dihydroxy -5,5 '-bistetrazole dihydroxy amine salt is 30%, 4, and the glycidyl amine type epoxy resin of 4 '-MDA four is
14.4%, epoxy resin E-51 are 5.47%, and o-tolyl glycidol ether is 13.03%, accelerator 0.5%, silicone resin
For 0.03%, diaminodiphenylsulfone is 6.57%.
The preparation method of above-mentioned oil/gas deep well high temperature resistant solid propellant, this method is followed the steps below：
Step one, according to formula rate, by high-temperature-resistant epoxy resin, bisphenol A epoxide resin, epoxide resin reactive diluent
For, accelerator boron trifluoride-amine complex, defoamer add mixing kettle in, premix 10 minutes；
Step 2, by weight percentage, addition potassium hyperchlorate, 1 into the system of step one, 1 '-dihydroxy -5,5 ' -
After bistetrazole dihydroxy amine salt is mixed 50 minutes, diaminodiphenylsulfone is added, mixing stops mixing after 15 minutes, obtains medicine slurry；
Step 3, medicine slurry is poured into mould, be put into 130 DEG C it is oven for curing, 72 hours, move back mould, obtain high temperature resistant
Solid propellant finished product.
Compared with prior art, beneficial has the technical effect that the present invention：
(1) solid propellant excellent hydrolysis resistance of the invention, 50mm × 50mm × 20mm medicine block in clear water and
Soaked in 3.5% salt solution up to 24~48 hours, weightlessness is less than 3%, and Volume Changes are less than 2%, do not occur significant change.And it is existing
The resistance to running water of solid propellant and 3.5% salt solution poor-performing.
(2) preferably, heatproof rank reaches 200 DEG C 48 hours to heat resistance of the present invention, does not occur spontaneous combustion, can be many in high temperature
Used in water environment.
Embodiment
Above-mentioned technical proposal is deferred to, following embodiments provide a kind of oil/gas deep well high temperature resistant solid propellant, with weight
Percentage meter：Potassium hyperchlorate is 30%~58%, 1,1 '-dihydroxy -5, and 5 '-bistetrazole dihydroxy amine salt is 2.00%~30%,
High-temperature-resistant epoxy resin is 10%~20.9%, and bisphenol A epoxide resin is 0~16.58%, and epoxide resin reactive diluent is
4.75~13.03%, accelerator boron trifluoride-amine complex is 0.5%, and defoamer is 0.03%, and diaminodiphenylsulfone is
6.57%~8.14%, raw material weight percentage summation is 100%, wherein：
Described bisphenol A epoxide resin is epoxy resin E-51；
Described high-temperature-resistant epoxy resin be the glycidyl amine type epoxy resin of 4,4 '-MDA four, 3,4 '-
The glycidyl amine type epoxy resin of diaminodiphenyl ether four or the glycidyl amine type epoxy resin of 4,4 '-diaminodiphenyl ether four；
Described epoxide resin reactive diluent is o-tolyl glycidol ether or polyethyleneglycol diglycidylether；
Described defoamer is silicone resin.
It is preferred that oil/gas deep well high temperature resistant solid propellant, by weight percentage, be made up of following raw material：Perchloric acid
Potassium is 30%, 1,1 '-dihydroxy -5, and 5 '-bistetrazole dihydroxy amine salt is 30%, 4, the glycidol of 4 '-MDA four
Amine type epoxy resin is 14.4%, and epoxy resin E-51 is 5.47%, and o-tolyl glycidol ether is 13.03%, accelerator
0.5%, silicone resin is 0.03%, and diaminodiphenylsulfone is 6.57%.
The specification requirement of above-mentioned raw materials is as follows：
1,1 '-dihydroxy -5,5 '-bistetrazole dihydroxy amine salt be industrial goods, yellow solid powder, granularity (1.5 μm of ＜) >=
92%, density 1.938g/cm3, acid number (PH) 4~7.Can be from triumphant examination (Shanghai) Science and Technology Ltd., Shanghai pottery Suo Shenghua sections
Skill Co., Ltd and spring westernization factory of Huixian City of Henan Province etc. purchase.1,1 '-dihydroxy -5,5 '-bistetrazole dihydroxy amine salt
(HATO) structural formula is as follows：
4, the glycidyl amine type epoxy resin of 4 '-MDA four (being abbreviated as TGDDM), rufous is to amber
Thick liquid, epoxide number >=0.8 equivalent/100g, 3.0~7.0Pas of viscosity (50 DEG C).TGDDM structural formula is as follows：
Epoxy resin E-51 epoxide number is 0.48~0.54,6.0~10.0Pas of viscosity (25 DEG C), polymerization degree n=
0.1~0.28, relative molecular mass is 307~420.Epoxy resin E-51 molecular formula is as follows：
O-tolyl glycidol ether outward appearance to be colourless to light yellow transparent liquid, epoxide number be 0.50~0.54 equivalent/
100g, 25 DEG C of viscositys are 5~10mPas.
Polyethyleneglycol diglycidylether outward appearance is to be colourless to light yellow transparent liquid, and epoxide number is worked as 0.30~0.36
Amount/100g, 25 DEG C of viscositys are 50~70mPas.
The viscosity of silicone resin is (100~1100) × 10-6m2/ s, refractive index nD 251.400~1.410.
The preparation method of above-mentioned oil/gas deep well high temperature resistant solid propellant, this method is followed the steps below：
Step one, according to formula rate, by weight percentage, by high-temperature-resistant epoxy resin be 10.00%~
20.90%, bisphenol A epoxide resin is 0~16.58%, and epoxide resin reactive diluent is 4.75~13.03%, accelerator three
Boron fluoride-amine complex is 0.50%, and defoamer is 0.03%, is added in mixing kettle, is premixed 10 minutes；
Step 2, by weight percentage, it is 30.00%~58.00% that potassium hyperchlorate is added into the system of step one,
1,1 '-dihydroxy -5,5 '-bistetrazole dihydroxy amine salt is 2.00%~30.00%, after mixing 50 minutes, adds diaminourea two
Benzene sulfone is 6.57%~8.14%, and mixing stops mixing after 15 minutes, obtains medicine slurry；
Step 3, the medicine slurry that step 2 is obtained is poured into mould, be put into 130 DEG C it is oven for curing, 72 hours, move back
Mould, obtains high temperature resistant solid propellant finished product.
Specific embodiment of the invention given below is, it is necessary to which explanation is that the invention is not limited in implement in detail below
Example, all equivalents done on the basis of technical scheme each fall within protection scope of the present invention.
Embodiment 1：
The oil/gas deep well of the present embodiment high temperature resistant solid propellant, by weight percentage, is made up of following raw material：It is high
Potassium chlorate is 30.00%, 1,1 '-dihydroxy -5, and 5 '-bistetrazole dihydroxy amine salt is 30.00%, 4,4 '-MDA
Four glycidyl amine type epoxy resins are 14.40%, and epoxy resin E-51 is 5.47%, and o-tolyl glycidol ether is
13.03%, accelerator boron trifluoride-amine complex is 0.50%, and silicone resin is 0.03%, and diaminodiphenylsulfone is
6.57%.
Performance test：
Quick-fried heat is determined by the quick-fried heat of GJB770B-2005 methods 701.2 and combustion heat constant temperature method.
Specific volume is determined by the specific volume pressure sensor method of GJB770B-2005 methods 702.1.
Heat-resisting quantity method of testing is：(1) 3 DEG C/min of Ф 20mm × 20mm powder columns rises to 200 DEG C, is incubated 48h；(2) control
Warm spot：Thermocouple is suspended from directly over sample, is not contacted with sample.Sample thermal weight loss is not more than 3%, and non-ignitable not quick-fried as pass through is tried
Test.
Propellant is water-fast, and method of testing is：50mm × 50mm × 20mm medicine blocks submerge 48h in running water, and weightlessness is less than
3%, Volume Changes are less than 2%, as pass through experiment.
The oil/gas deep well of the present embodiment is shown in Table 1 with the properties test result of high temperature resistant solid propellant.
The properties test result of 1 embodiment of table 1
As can be drawn from Table 1, quick-fried hot (i.e. the energy) of the propellant is slightly higher, and specific volume is moderate, and resistance to elevated temperatures, water-fast
Performance and resistance to salt water can reach performance requirement.It is adapted to the heat-resisting Pressure breaking bullet powder charge of oil/gas deep well to use.
Embodiment 2：
The oil/gas deep well of the present embodiment high temperature resistant solid propellant, by weight percentage, is made up of following raw material：It is high
Potassium chlorate is that 35.00%, HATO is that 25.00%, TGDDM is 10.00%, and epoxy resin E-51 is 16.58%, o-tolyl contracting
Water glycerin ether is 4.75%, and accelerator boron trifluoride-amine complex is 0.50%, and silicone resin is 0.03%, diaminourea hexichol
Sulfone is 8.14%.
The oil/gas deep well of the present embodiment is same as Example 1 with the performance test methods of high temperature resistant solid propellant, every
The performance test results are shown in Table 2.
The properties test result of 2 embodiment of table 2
As can be drawn from Table 2, quick-fried hot (i.e. the energy) of the propellant is moderate, and specific volume is moderate, and resistance to elevated temperatures, water-fast
Performance and resistance to salt water can reach performance requirement.It is adapted to the heat-resisting Pressure breaking bullet powder charge of oil/gas deep well to use.
Embodiment 3：
The oil/gas deep well of the present embodiment high temperature resistant solid propellant, by weight percentage, is made up of following raw material：It is high
Potassium chlorate is that 58.00%, HATO is that 2.00%, TGDDM is 20.90%, and o-tolyl glycidol ether is 11.25%, is promoted
Agent boron trifluoride-amine complex is 0.50%, and silicone resin is 0.03%, and diaminodiphenylsulfone is 7.32%.
The oil/gas deep well of the present embodiment is same as Example 1 with the performance test methods of high temperature resistant solid propellant, every
The performance test results are shown in Table 3.
The properties test result of 3 embodiment of table 3
As can be drawn from Table 3, quick-fried hot (i.e. the energy) of the propellant is moderate, and specific volume is moderate, and resistance to elevated temperatures, water-fast
Performance and resistance to salt water can reach performance requirement.The heat-resisting Pressure breaking bullet powder charge of oil/gas deep well also is adapted for use.
In all of above embodiment, raw material o-tolyl glycidol ether can be replaced with polyethyleneglycol diglycidylether
Change, raw material 4, the glycidyl amine type epoxy resin of 4 '-MDA four (being abbreviated as TGDDM) can use 3,4 '-diamino
The glycidyl amine type epoxy resin of yl diphenyl ether four (being abbreviated as 3,4 '-TGDDE) or the glycidol of 4,4 '-diaminodiphenyl ether four
Amine type epoxy resin (being abbreviated as 4,4 '-TGDDE) is replaced, and technique effect is identical, in view of length, will no longer provide corresponding one by one
Embodiment.
Claims (2)
1. a kind of oil/gas deep well high temperature resistant propellant, it is characterised in that by weight percentage, is made up of following raw material：It is high
Potassium chlorate is 58.00%, 1,1 '-dihydroxy -5, and 5 '-bistetrazole dihydroxy amine salt is 2.00%, 4,4 '-MDA four
Glycidyl amine type epoxy resin is 20.90%, and o-tolyl glycidol ether is 11.25%, and boron trifluoride-amine complex is
0.50%, silicone resin is 0.03%, and diaminodiphenylsulfone is 7.32%；
Obtained oil/gas deep well carries out heat-resisting quantity test with high temperature resistant propellant at 200 DEG C, is incubated 48h, the heat mistake of sample
Weight is 1.5%.
2. the oil/gas deep well as claimed in claim 1 preparation method of high temperature resistant propellant, it is characterised in that this method according to
Following steps are carried out：
Step one, according to formula rate, by the glycidyl amine type epoxy resin of 4,4 '-MDA four, o-tolyl
Glycidol ether, boron trifluoride-amine complex, silicone resin are added in mixing kettle, are premixed 10 minutes；
Step 2, potassium hyperchlorate, 1 are added into mixing kettle, and 1 '-dihydroxy -5,5 '-bistetrazole dihydroxy amine salt is mixed 50 minutes
Afterwards, diaminodiphenylsulfone is added, mixing stops mixing after 15 minutes, obtains medicine slurry；
Step 3, medicine slurry is poured into mould, be put into 130 DEG C it is oven for curing, 72 hours, move back mould, obtain high temperature resistant solid
Propellant finished product.
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