CN106632955A - Hydroxy terminated polybutadiene propellant grain defect repairing material and application technique thereof - Google Patents

Hydroxy terminated polybutadiene propellant grain defect repairing material and application technique thereof Download PDF

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Publication number
CN106632955A
CN106632955A CN201611173157.XA CN201611173157A CN106632955A CN 106632955 A CN106632955 A CN 106632955A CN 201611173157 A CN201611173157 A CN 201611173157A CN 106632955 A CN106632955 A CN 106632955A
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China
Prior art keywords
repair
powder column
container
carbon black
repair materials
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CN201611173157.XA
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Chinese (zh)
Inventor
张文奎
芮振洋
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INNER MONGOLIA SPACE HONGXIA CHEMICAL Co Ltd
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INNER MONGOLIA SPACE HONGXIA CHEMICAL Co Ltd
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Priority to CN201611173157.XA priority Critical patent/CN106632955A/en
Publication of CN106632955A publication Critical patent/CN106632955A/en
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C08G18/62—Polymers of compounds having carbon-to-carbon double bonds
    • C08G18/6204—Polymers of olefins
    • C—CHEMISTRY; METALLURGY
    • C06—EXPLOSIVES; MATCHES
    • C06D—MEANS FOR GENERATING SMOKE OR MIST; GAS-ATTACK COMPOSITIONS; GENERATION OF GAS FOR BLASTING OR PROPULSION (CHEMICAL PART)
    • C06D5/00—Generation of pressure gas, e.g. for blasting cartridges, starting cartridges, rockets
    • C06D5/06—Generation of pressure gas, e.g. for blasting cartridges, starting cartridges, rockets by reaction of two or more solids
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/30—Low-molecular-weight compounds
    • C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
    • C08G18/3203—Polyhydroxy compounds
    • C08G18/3206—Polyhydroxy compounds aliphatic
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
    • C08G18/72—Polyisocyanates or polyisothiocyanates
    • C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
    • C08G18/76—Polyisocyanates or polyisothiocyanates cyclic aromatic
    • C08G18/7614—Polyisocyanates or polyisothiocyanates cyclic aromatic containing only one aromatic ring
    • C08G18/7621—Polyisocyanates or polyisothiocyanates cyclic aromatic containing only one aromatic ring being toluene diisocyanate including isomer mixtures
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/02—Elements
    • C08K3/04—Carbon
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/16—Nitrogen-containing compounds
    • C08K5/17—Amines; Quaternary ammonium compounds
    • C08K5/18—Amines; Quaternary ammonium compounds with aromatically bound amino groups
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2296—Oxides; Hydroxides of metals of zinc

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Engineering & Computer Science (AREA)
  • Combustion & Propulsion (AREA)

Abstract

The invention aims at repairing cured hydroxy terminated polybutadiene propellant grain physical defects and achieving the technical purpose of achieving a combustible repairing material capable of being cured at room temperature. A hydroxy terminated polybutadiene and toluene diisocynate crosslinking and curing system which is the same as a curing adhesive system of an original propellant is adopted, and formula components comprise hydroxy terminated polybutadiene, toluene diisocynate, glycerol, zinc oxide, carbon black, 2,4,6-tri-(dimethylamine methyl)phenol and cured propellant powder needing to be prepaired; the ratio of the isocyanate group equivalent of toluene diisocynate to the hydroxyl equivalent of hydroxy terminated polybutadiene is 0.9-1.2. The repairing material can be cured at room temperature and combust, and a making and using method of the repairing material comprises 11 steps.

Description

A kind of htpb solid propellant powder column defect repair material and its application technology
Technical field
The present invention relates to solid propellant rocket manufacturing technology, more particularly to solid propellant rocket propellant charge defect Recovery technique.
Background technology
In solid propellant rocket manufacturing technology field, fourth hydroxyl formula solid propellant is the most frequently used propulsion both at home and abroad at present Agent.However, in solid propellant rocket manufacture process, solid propellant grain usually occurs that a range of physics lacks Fall into.The change of the time-pressure curve when presence of the defect will cause solid propellant rocket to work, when defect exceeds During certain limit value, time-pressure curve will cause solid propellant rocket work failure beyond design permissible range.Cause This, when defect exceedes the certain limit value of design code, it is desirable to repaired.At present, for fourth hydroxyl formula solid propellant Powder column physical imperfection, the repair materials for being adopted mainly are unable to incendiary material and can be with incendiary material.Using the material that can not burn Material repairs powder column defect, and powder column incipient combustion surface reduces compared with design load after causing to repair, and can adopt when defect is small.Using Energy incendiary material repairs powder column defect, and powder column incipient combustion surface reduces not enough compared with design load after the reparation that can effectively take on a new look.Boat Its technique fifth phase page 10 in 1997 describes the whole machine maintenance recovering technology of composite solidpropellant, it is disclosed that for repairing Three binder formulas that can be burnt of the htpb solid propellant defect of solidification, and the binder formula is needed at high temperature Can solidification.For cured solid propellant grain, secondary high-temperature solidification will cause powder column intensity to rise, under elongation percentage Drop.
The content of the invention
The present invention is directed to cured htpb solid propellant powder column physical imperfection, and solution is required to normal temperature cure and flammable The technical problem of the repair materials of burning.In the present invention, using poly- with former propellant curing adhesive composition identical terminal hydroxy group Butadiene+toluene di-isocyanate(TDI) crosslinking curing system, is conducive to repair materials crosslinking bonding with cured solid propellant, protects Card adhesive strength；In end hydroxy butadiene+toluene di-isocyanate(TDI) crosslinking curing system, the isocyanic acid of toluene di-isocyanate(TDI) There is chemical reaction in the hydroxyl of ester group and end hydroxy butadiene, determine the mechanical property of repair materials；Employing in formula need to be repaiied Solidifying COMPOSITE SOLID PROPELLANT end again can make repair materials incendivity, while being also relatively beneficial to improve the mechanical property after repair materials solidification Energy；The color of repair materials can be effectively adjusted in formula using carbon black, makes powder column repair surface with former propellant surface colour-difference It is attractive in appearance away from little, while being also combustible species.
In material prescription is repaired, experiment shows, the parameter that can solidify is the NCO of toluene di-isocyanate(TDI) Equivalent：Hydroxyl equivalent=0.85～1.25 of end hydroxy butadiene；Optimal equivalent proportion is 0.9～1.2；In winter-spring season, equivalent Than for 0.9～1.0, preferably；In summer and autumn, equivalent proportion is 1.0～1.2, preferably.
According to the different propellant charges to be repaired, repair materials weight proportion scope：End hydroxy butadiene+first Phenylene diisocyanate, 105～110 parts；Glycerine, 0.45 part；Zinc oxide, 60～160 parts；Carbon black, 1.5～3.0 parts；2,4, 6- tri--（Dimethylamino methyl）Phenol, 0.5～1.0 part；Solidification COMPOSITE SOLID PROPELLANT need to be repaired last, 40 parts.More conventional weight is matched somebody with somebody Compare scope：End hydroxy butadiene+toluene di-isocyanate(TDI), 106～108 parts；Glycerine, 0.45 part；Zinc oxide, 80～120 Part；Carbon black, 1.5～3.0 parts；2,4,6- tri--（Dimethylamino methyl）Phenol, 0.7～0.9 part；Solidification COMPOSITE SOLID PROPELLANT need to be repaired End, 40 parts.
Repair materials make using method, comprise the steps：
Step one, will need the rejected region for repairing propellant charge to be trimmed to range estimation without wedge angle, repair materials material with dressing blade Slurry is easy to the shape filled；A small amount of absolute ethyl alcohol is dipped in byssus to clean out rejected region, dry naturally no less than 30 points Clock；
Step 2, it would be desirable to which the cured propellant medicine block for repairing powder column frustrates into unqualified, 24 mesh sieves excessively, loads ready appearance In device；
Step 3, it would be desirable to carbon black, cross 40 mesh sieves, in being fitted into ready container；
Step 4, it would be desirable to toluene di-isocyanate(TDI) exist（17～38）More than 48 hours are incubated under the conditions of DEG C；
Step 5, it would be desirable to zinc oxide held with enamel tray, being put into temperature is（120±10）DEG C baking oven in dried, Drying time is no less than 7 hours, and 80 mesh sieves are crossed in 4 hours afterwards, deposits in drier, should use in 72 hours；
Step 6, according to the consumption of repair materials recipe calculation, determines end hydroxy butadiene usage amount and proportion container, by end Hydroxyl polybutadiene is weighed in container；Zinc oxide is weighed in container again, gradation feed postition is used in zinc oxide charging, will with hammer drill End hydroxy butadiene and zinc oxide stir；Glycerine is added in container again, is stirred with hammer drill；Again by 2,4,6- Three-（Dimethylamino methyl）Phenol is added in container, is stirred with hammer drill, forms slip；
Step 7, in the slip in the container of step 6, adds the ready medicine end of step 2, is stirred with hammer drill；
Step 8, in the slip in the container of step 7, adds the ready carbon black of step 3, is gradually added on a small quantity, on one side Plus while stirred with hammer drill, while estimating slip and the propellant charge or medicine block color contrast that need to repair, work as range estimation During solid colour, stop adding carbon black, stirred with hammer drill；
Step 9, in the slip in the container of step 8, adds the ready toluene two by recipe calculation amount of step 4 different Cyanate, is stirred with hammer drill；
Step 10, the reparation slip for being prepared step 9 with shovel fills propellant charge rejected region, will insert defective part The slip compacting of position；Non- shaping surface requires that repair materials are concordant and smooth with powder column type face, and shaping surface requires that repair materials are higher by Powder column type face（1～5）Millimeter；
Step 11, after propellant charge defect repair, after normal temperature cure 24 hours, defect, will with sand paper in non-shaping surface The repair materials polishing of rejected region is smooth, dips in a small amount of absolute ethyl alcohol with byssus and puts rejected region painting and grain surface face on the skin Semu is surveyed and is close to；Defect shaping surface with dressing blade by the unnecessary repair materials that rejected region is higher by powder column type face be trimmed to Powder column type face is concordant.

Claims (5)

1. a kind of htpb solid propellant powder column defect repair material, it is characterised in that repair materials formula constituent includes end hydroxyl Base polybutadiene, toluene di-isocyanate(TDI), glycerine, zinc oxide, carbon black, 2,4,6- tri--（Dimethylamino methyl）Phenol, need to repair Solidify COMPOSITE SOLID PROPELLANT end again.
2. a kind of htpb solid propellant powder column defect repair material according to claim 1, it is characterised in that described to repair In multiple material prescription component, the NCO equivalent of toluene di-isocyanate(TDI)：Hydroxyl equivalent=0.9 of end hydroxy butadiene ～1.2.
3. a kind of htpb solid propellant powder column defect repair material according to claim 2, it is characterised in that described to repair Again material weight proportioning is：End hydroxy butadiene+toluene di-isocyanate(TDI), 105～110 parts；Glycerine, 0.45 part；Oxidation Zinc, 60～160 parts；Carbon black, 1.5～3.0 parts；2,4,6- tri--（Dimethylamino methyl）Phenol, 0.5～1.0 part；Need to repair solid Change COMPOSITE SOLID PROPELLANT last, 40 parts.
4. a kind of htpb solid propellant powder column defect repair material according to claim 3, it is characterised in that described to repair The proportioning consumption of carbon black in multiple material, is determined by observing the color of the repair materials, when adding carbon in the repair materials When black amount causes the color of repair materials identical with the color ready visual contrast of the propellant charge that need to be repaired, the addition carbon black Measure as the proportioning consumption of carbon black in repair materials.
5. user is made according to a kind of arbitrary described htpb solid propellant powder column defect repair material of Claims 1 to 4 Method, its feature comprises the steps：
Step one, will need the rejected region for repairing propellant charge to be trimmed to range estimation without wedge angle, repair materials material with dressing blade Slurry is easy to the shape filled；A small amount of absolute ethyl alcohol is dipped in byssus to clean out rejected region, dry naturally no less than 30 points Clock；
Step 2, it would be desirable to which the cured propellant medicine block for repairing powder column frustrates into unqualified, 24 mesh sieves excessively, loads ready appearance In device；
Step 3, it would be desirable to carbon black, cross 40 mesh sieves, in being fitted into ready container；
Step 4, it would be desirable to toluene di-isocyanate(TDI) exist（17～38）More than 48 hours are incubated under the conditions of DEG C；
Step 5, it would be desirable to zinc oxide held with enamel tray, being put into temperature is（120±10）DEG C baking oven in dried, Drying time is no less than 7 hours, and 80 mesh sieves are crossed in 4 hours afterwards, deposits in drier, should use in 72 hours；
Step 6, according to the consumption of repair materials recipe calculation, determines end hydroxy butadiene usage amount and proportion container, by end Hydroxyl polybutadiene is weighed in container；Zinc oxide is weighed in container again, gradation feed postition is used in zinc oxide charging, will with hammer drill End hydroxy butadiene and zinc oxide stir；Glycerine is added in container again, is stirred with hammer drill；Again by 2,4,6- Three-（Dimethylamino methyl）Phenol is added in container, is stirred with hammer drill, forms slip；
Step 7, in the slip in the container of step 6, adds the ready medicine end of step 2, is stirred with hammer drill；
Step 8, in the slip in the container of step 7, adds the ready carbon black of step 3, is gradually added on a small quantity, on one side Plus while stirred with hammer drill, while estimating slip and the propellant charge or medicine block color contrast that need to repair, work as range estimation During solid colour, stop adding carbon black, stirred with hammer drill；
Step 9, in the slip in the container of step 8, adds the ready toluene two by recipe calculation amount of step 4 different Cyanate, is stirred with hammer drill；
Step 10, the reparation slip for being prepared step 9 with shovel fills propellant charge rejected region, will insert defective part The slip compacting of position；Non- shaping surface requires that repair materials are concordant and smooth with powder column type face, and shaping surface requires that repair materials are higher by Powder column type face（1～5）Millimeter；
Step 11, after propellant charge defect repair, after normal temperature cure 24 hours, defect, will with sand paper in non-shaping surface The repair materials polishing of rejected region is smooth, dips in a small amount of absolute ethyl alcohol with byssus and puts rejected region painting and grain surface face on the skin Semu is surveyed and is close to；Defect shaping surface with dressing blade by the unnecessary repair materials that rejected region is higher by powder column type face be trimmed to Powder column type face is concordant.
CN201611173157.XA 2016-12-18 2016-12-18 Hydroxy terminated polybutadiene propellant grain defect repairing material and application technique thereof Pending CN106632955A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107384294A (en) * 2017-07-24 2017-11-24 湖北三江航天江河化工科技有限公司 A kind of grouting material and preparation method thereof
CN108456293A (en) * 2018-03-13 2018-08-28 中国人民解放军国防科技大学 Composite solid propellant grain defect repairing material and preparation method thereof
KR20220031229A (en) * 2020-09-04 2022-03-11 주식회사 한화 Solid propellant repair washcoat composition and solid propellant repair method

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107384294A (en) * 2017-07-24 2017-11-24 湖北三江航天江河化工科技有限公司 A kind of grouting material and preparation method thereof
CN108456293A (en) * 2018-03-13 2018-08-28 中国人民解放军国防科技大学 Composite solid propellant grain defect repairing material and preparation method thereof
KR20220031229A (en) * 2020-09-04 2022-03-11 주식회사 한화 Solid propellant repair washcoat composition and solid propellant repair method
KR102575547B1 (en) 2020-09-04 2023-09-11 한화에어로스페이스 주식회사 Solid propellant repair washcoat composition and solid propellant repair method

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