CN109053342A - A kind of preparation method for the medicine slurry that no bonding agent is precipitated - Google Patents

A kind of preparation method for the medicine slurry that no bonding agent is precipitated Download PDF

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Publication number
CN109053342A
CN109053342A CN201810704970.8A CN201810704970A CN109053342A CN 109053342 A CN109053342 A CN 109053342A CN 201810704970 A CN201810704970 A CN 201810704970A CN 109053342 A CN109053342 A CN 109053342A
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end hydroxy
premix
diethanol amine
complex compound
hydroxy butadiene
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CN201810704970.8A
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CN109053342B (en
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张博
沈明
韩晓娟
张武卫
曹巍
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Xi'an Aerospace Chemical Power Co Ltd
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Xi'an Aerospace Chemical Power Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C06EXPLOSIVES; MATCHES
    • C06BEXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
    • C06B27/00Compositions containing a metal, boron, silicon, selenium or tellurium or mixtures, intercompounds or hydrides thereof, and hydrocarbons or halogenated hydrocarbons

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)

Abstract

A kind of preparation method for the medicine slurry that no bonding agent is precipitated, by end hydroxy butadiene and diethanol amine melamine complex compound 50 DEG C ± 10 DEG C preliminary drying 12 hours or more, to reduce the viscosity of end hydroxy butadiene Yu diethanol amine melamine complex compound;By a small amount of, multiple premix, is gradually blended with sticky material with end hydroxy butadiene, progressively reach and premixed uniform purpose;End hydroxy butadiene and the pre- mixed slurry of diethanol amine melamine complex compound are poured into addition other raw material premix material container internal reference and add premix, is sufficiently stirred evenly.The present invention utilizes the existing hardware facility of process, by preparing raw material, the analysis of the premixing process of medicine slurry and raw material physicochemical characteristics etc., grope, improve technique, it ensure that the uniformity for weighing process premix medicine slurry, with strong operability, and it is almost the same to premix out the medicine slurry uniformity, ensure that medicine slurry quality.

Description

A kind of preparation method for the medicine slurry that no bonding agent is precipitated
Technical field
The present invention relates to solid propellant rocket field, the preparation method for the medicine slurry that specifically a kind of no bonding agent is precipitated.
Background technique
In the production process of certain model solid propellant rocket, repeatedly there is black powder position, brown spot, send mixing Material container after the cleaning of post has a small amount of diethanol amine melamine complex compound adherency, diethanol amine melamine complex compound difficult With it is fully premixed uniform the problems such as, seriously affected the product quality and manufacturing schedule of powder column.
Existing technology is: by technique requirement, viscosity is greater than the bonding agent diethanol amine melamine of 20pa.s by when premix Amine complex is all added in end hydroxy butadiene, and other components are then added, then carries out stirring premix by hand, due to diethyl After hydramine melamine complex compound is added in end hydroxy butadiene, thin pulp bottom is sunk to quickly, it is additional to expect during transportation Container bottom and transport vehicle Contact Temperature are lower, cause the precipitation of diethanol amine melamine complex compound to be adhered to container bottom, no It can guarantee raw material charging precision.In addition, diethanol amine melamine complex compound and end hydroxy butadiene premix after, material with The contact surface of material container can all have dark-brown dough precipitating, can not be stirred evenly the dough of deposition with bamboo shovel.Cause original Material cannot be added completely into medicine slurry, and medicine slurry mixing unevenly leads to the problem of grain surface spot, there are biggish hidden danger of quality, Seriously affect the delivery progress of powder column.
Diethanol amine melamine complex compound disperses problem of non-uniform, the method used in the prior art when for premix Are as follows:
Original process one: 1 weigh diethanol amine melamine complex compound in rustless steel container, with the poly- fourth of the terminal hydroxy group being baked Diene covers diethanol amine melamine complex compound and stirring once, is then placed within 50 DEG C of ± 10 DEG C of baking 12h or more by hand. 2, first slurry is again stirring on the day of feeding intake, premix slurry is then poured into 1000L premix material container internal reference and adds premix.
Original process two: 1 weigh diethanol amine melamine complex compound in rustless steel container, and it is poly- to weigh the terminal hydroxy group being baked The covering of diethanol amine melamine complex compound is placed on 50 DEG C of ± 10 DEG C of baking 12h or more by butadiene.2, feeding intake the same day first will material Then slurry stirring premixes the addition of other load weighted components.
But after implementing above two technique, the contact surface of material and material container can all have dark-brown diethanol amine melamine Complex compound dough precipitating, and particle is uneven, is again stirring for rear particle and is all suspended in slurry, can not reach uniform mixing Purpose.
Summary of the invention
To overcome the problems, such as grain surface spot existing in the prior art and there are hidden danger of quality, the invention proposes one The preparation method for the medicine slurry that kind is precipitated without bonding agent.
The component for the medicine slurry that no bonding agent is precipitated are as follows: 0.1% diethanol amine melamine complex compound, 10% octyl two Luxuriant iron, 5% N-N ' diphenyl-para-phenylene diamine, 10% industrial Kui diacid di-isooctyl, 19.9% ball-type aluminium powder and 55% End hydroxy butadiene.The percentage is mass percent.
Detailed process of the invention is:
Step 1, preliminary drying.The diethanol amine melamine complex compound of colloidal substance and thick end hydroxy butadiene is same When be placed in heating 12~24 hours in 50 DEG C of ± 10 DEG C of drying chambers, it is poly- to reduce the diethanol amine melamine complex compound and terminal hydroxy group The viscosity of butadiene.
Step 2, mixing.It will be pre- by the diethanol amine melamine complex compound of preliminary drying and end hydroxy butadiene premix Mixing slurry.The mixing is mixed three times and is completed in 50 DEG C ± 10 DEG C of drying chamber by mixing three times.
I point of end hydroxy butadiene: being divided into four parts for the end hydroxy butadiene that the content is referred to as 55%, divides in preparation Secondary addition.
In four parts of end hydroxy butadienes: first part of end hydroxy butadiene of weighing: diethanol amine melamine Complex compound=0.5:1;The second part of end hydroxy butadiene weighed: diethanol amine melamine complex compound=1:1;The weighed Three parts of end hydroxy butadienes: diethanol amine melamine complex compound=1:1;Surplus is the 4th part.The ratio is weight Than.
II is placed in load weighted diethanol amine melamine complex compound in premix material container, by first part of end hydroxyl of weighing Base polybutadiene is added in premix material container, and diethanol amine melamine complex compound is covered;And it is thoroughly mixed It is even, the viscosity of diethanol amine melamine complex compound is dispersed by end hydroxy butadiene.Obtain mixed mixing for the first time Object.
III second part of end hydroxy butadiene of weighing is added in premix material container, with the first time in premix material container Mixed mixture is thoroughly mixed uniformly again, by second part of end hydroxy butadiene being added again by diethanol Amine melamine mixture is completely dispersed.Obtain second of mixed mixture.
IV third part end hydroxy butadiene of weighing is added in premix material container, with second in premix material container Mixed mixture is thoroughly mixed uniformly again.
So far, mixing three times is completed, premix slurry is obtained.
Step 3, octyl ferrocene, N-N ' diphenyl-para-phenylene diamine, industrial Kui diacid two are weighed by the medicine slurry component of design Different monooctyl ester, ball-type aluminium powder.By load weighted octyl ferrocene, N-N ' diphenyl-para-phenylene diamine, industrial Kui diacid di-isooctyl, ball Type aluminium powder is placed in mixing vessel, and is stirred evenly after end hydroxy butadiene is added, and premix slurry and the poly- fourth of terminal hydroxy group are obtained The mixture of diene.The ratio of the component of the additional amount of the end hydroxy butadiene and the design is terminal hydroxy group polybutadiene Alkene: component=50 of design~80:1;The ratio is weight ratio.
Obtained premix slurry is added in the mixture of the high viscosity raw material and end hydroxy butadiene, is sufficiently stirred It mixes and uniformly obtains the medicine slurry that uniformly mixed no bonding agent is precipitated.
The present invention overcomes diethanol amine melamine complex compound raw material viscosity is larger, premixed with other raw material uneven Even problem provides premix uniform medicine slurry for rear process.
For the deficiencies in the prior art, the present invention does following improvement:
1, preliminary drying end hydroxy butadiene and diethanol amine melamine complex compound 12 hours or more (50 DEG C of drying room temperature ± 10℃);To reduce the viscosity of end hydroxy butadiene Yu diethanol amine melamine complex compound.
2, a small amount of, repeatedly manual to premix, it is gradually blended, is progressively reached it with sticky material with end hydroxy butadiene Premix uniform purpose.
3, then end hydroxy butadiene and the pre- mixed slurry of diethanol amine melamine complex compound are poured into and it is added He adds premix by raw material premix material container internal reference, sufficiently stirs evenly;Uniform purpose is premixed to reach medicine slurry.
The actual production effect of premixing process after optimization shows:
1, new premixing process is able to solve the precipitation of diethanol amine melamine complex compound and is adhered to material container bottom and work Problem on tool, premixing effect are good;
2, it premixes in medicine slurry and is precipitated without diethanol amine melamine complex granulation suspended matter, medicine slurry each component sufficiently melts It closes;
3, since new premixing process is implemented, do not occurred powder column apparent mass problem.
The present invention utilizes the existing hardware facility of process (container, drying chamber, material preparation method), by raw material standard The analysis of standby, medicine slurry premixing process and raw material physicochemical characteristics etc. is groped, and is improved technique, be ensure that weighing work The uniformity of sequence premix medicine slurry.Meanwhile strong operability of the present invention, and it is almost the same to premix out the medicine slurry uniformity, ensure that Medicine slurry quality.
Detailed description of the invention
Fig. 1 is that diethanol amine melamine complex compound and end hydroxy butadiene premix are uneven, appears in powder position Black, brown spot.
Fig. 2 is that the precipitation of diethanol amine melamine complex compound is adhered to container bottom, illustrates that original process method cannot be guaranteed Raw material charging precision.
Fig. 3 is the precipitating bulk being adhered on container in the diethanol amine melamine complex compound obtained using original process Object, the non-uniform phenomenon of particle.
Fig. 4 is the precipitating dough in the diethanol amine melamine complex compound obtained using original process, is particle unevenness Even phenomenon.
Fig. 5 is the slurry in the present invention after first time mixing.
Fig. 6 is that premix slurry is obtained after completing mixing three times in the present invention.
Fig. 7 is flow chart of the invention.
Specific embodiment
The present embodiment is a kind of preparation method of medicine slurry that no bonding agent is precipitated.
The component of the present embodiment medicine slurry are as follows: 0.1% diethanol amine melamine complex compound, 10% octyl ferrocene, 5% N-N ' diphenyl-para-phenylene diamine, 10% industrial Kui diacid di-isooctyl, 19.9% ball-type aluminium powder and 55% end hydroxyl Base polybutadiene.The percentage is mass percent.
The detailed process of the present embodiment is:
Step 1, preliminary drying.
The diethanol amine melamine complex compound of colloidal substance and thick end hydroxy butadiene are placed in 50 DEG C simultaneously Heating 12~24 hours in ± 10 DEG C of drying chambers, to reduce the viscous of the diethanol amine melamine complex compound and end hydroxy butadiene Consistency.
Step 2, mixing.
It will be by the diethanol amine melamine complex compound of preliminary drying and end hydroxy butadiene premix premix slurry.Described Mixing is mixed three times and is completed in 50 DEG C ± 10 DEG C of drying chamber by mixing three times.
Specifically:
I point of end hydroxy butadiene: being divided into four parts for the end hydroxy butadiene that the content is referred to as 55%, divides in preparation Secondary addition.In four parts of end hydroxy butadienes: first part of end hydroxy butadiene of weighing: diethanol amine melamine network Close object=0.5:1;The second part of end hydroxy butadiene weighed: diethanol amine melamine complex compound=1:1;The third of weighing Part end hydroxy butadiene: diethanol amine melamine complex compound=1:1;Surplus is the 4th part.The ratio is weight ratio. The diethanol amine melamine complex compound is bonding agent, and viscosity is greater than 20pa.s.
II is placed in load weighted diethanol amine melamine complex compound in premix material container, by first part of end hydroxyl of weighing Base polybutadiene is added in premix material container, and diethanol amine melamine complex compound is covered;It is thoroughly mixed uniformly, Disperse the viscosity of diethanol amine melamine complex compound by end hydroxy butadiene.Obtain mixed mixture for the first time.
III second part of end hydroxy butadiene of weighing is added in premix material container, with the first time in premix material container Mixed mixture is thoroughly mixed uniformly again, by second part of end hydroxy butadiene being added again by diethanol Amine melamine mixture is completely dispersed.Obtain second of mixed mixture.
IV third part end hydroxy butadiene of weighing is added in premix material container, with second in premix material container Mixed mixture is thoroughly mixed uniformly again.
So far, mixing three times is completed, premix slurry is obtained.
Step 3, medicine slurry is prepared.
By the medicine slurry component of design weigh octyl ferrocene, N-N ' diphenyl-para-phenylene diamine, industrial Kui diacid di-isooctyl, Ball-type aluminium powder and end hydroxy butadiene.By load weighted octyl ferrocene, N-N ' diphenyl-para-phenylene diamine, industrial Kui diacid two Different monooctyl ester, ball-type aluminium powder are placed in mixing vessel, are stirred evenly, are obtained pre- after remaining 4th part of end hydroxy butadiene is added The mixture of mixing slurry and end hydroxy butadiene.
Obtained premix slurry is added in the mixture of the high viscosity raw material and end hydroxy butadiene, is sufficiently stirred It mixes and uniformly obtains the medicine slurry that uniformly mixed no bonding agent is precipitated.

Claims (4)

1. a kind of preparation method for the medicine slurry that no bonding agent is precipitated, the component of medicine slurry are as follows: 0.1% diethanol amine melamine network Close object, 10% octyl ferrocene, 5% N-N ' diphenyl-para-phenylene diamine, 10% industrial Kui diacid di-isooctyl, 19.9% Ball-type aluminium powder and 55% end hydroxy butadiene;The percentage is mass percent;
It is characterized in that, detailed process is:
Step 1, preliminary drying;
Step 2, it mixing: will premix by the diethanol amine melamine complex compound and end hydroxy butadiene of preliminary drying as premix Slurry;The mixing is mixed three times and is completed in 50 DEG C ± 10 DEG C of drying chamber by mixing three times;
Step 3, it prepares medicine slurry: weighing octyl ferrocene, N-N ' diphenyl-para-phenylene diamine, industrial Kui two by the medicine slurry component of design Sour di-isooctyl, ball-type aluminium powder;Load weighted octyl ferrocene, N-N ' diphenyl-para-phenylene diamine, industrial Kui diacid two is different pungent Ester, ball-type aluminium powder are placed in mixing vessel, and are stirred evenly after end hydroxy butadiene is added, and premix slurry and terminal hydroxy group are obtained The mixture of polybutadiene;The ratio of the component of the additional amount of the end hydroxy butadiene and the design is the poly- fourth of terminal hydroxy group Diene: component=50 of design~80:1;The ratio is weight ratio;
Obtained premix slurry is added in the mixture of the high viscosity raw material and end hydroxy butadiene, is sufficiently stirred It is even, obtain the medicine slurry that uniformly mixed no bonding agent is precipitated.
2. the preparation method for the medicine slurry being precipitated as described in claim 1 without bonding agent, which is characterized in that step 2 mixing Detailed process is:
I point of end hydroxy butadiene: being divided into four parts for the end hydroxy butadiene that the content is referred to as 55%, adds by several times in preparation Enter;
II is placed in load weighted diethanol amine melamine complex compound in premix material container, and first part of terminal hydroxy group of weighing is gathered Butadiene is added in premix material container, and diethanol amine melamine complex compound is covered;And be thoroughly mixed uniformly, lead to Cross the viscosity of end hydroxy butadiene dispersion diethanol amine melamine complex compound;Obtain mixed mixture for the first time;
III second part of end hydroxy butadiene of weighing is added in premix material container, mixes with the first time in premix material container Mixture afterwards is thoroughly mixed uniformly again, by second part of end hydroxy butadiene being added again by diethanol amine three Poly cyanamid mixture is completely dispersed;Obtain second of mixed mixture;
IV third part end hydroxy butadiene of weighing is added in premix material container, mixes with second in premix material container Mixture afterwards is thoroughly mixed uniformly again;
So far, mixing three times is completed, premix slurry is obtained.
3. the preparation method for the medicine slurry being precipitated as claimed in claim 2 without bonding agent, which is characterized in that four parts of terminal hydroxy groups are poly- In butadiene: first part of end hydroxy butadiene of weighing: diethanol amine melamine complex compound=0.5:1;Second weighed Part end hydroxy butadiene: diethanol amine melamine complex compound=1:1;Third part end hydroxy butadiene of weighing: diethyl Hydramine melamine complex compound=1:1;Surplus is the 4th part;The ratio is weight ratio.
4. the preparation method for the medicine slurry being precipitated as described in claim 1 without bonding agent, which is characterized in that the preliminary drying is by colloid The diethanol amine melamine complex compound and thick end hydroxy butadiene of shape, which are placed in simultaneously in 50 DEG C of ± 10 DEG C of drying chambers, to be added Heat 12~24 hours, to reduce the viscosity of the diethanol amine melamine complex compound and end hydroxy butadiene.
CN201810704970.8A 2018-03-12 2018-07-02 Preparation method of medicinal slurry without bonding agent precipitation Active CN109053342B (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101113123A (en) * 2007-07-16 2008-01-30 上海东方久乐汽车安全气囊有限公司 Multiple micro-porous gas production charge column and method for making same
DE102007029644A1 (en) * 2007-06-26 2009-01-08 Henkel Ag & Co. Kgaa One-component, hot-curing reactive composition
US20130048163A1 (en) * 2011-08-31 2013-02-28 Alliant Techsystems Inc. Propellant compositions including stabilized red phosphorus, a method of forming same, and an ordnance element including the same
CN102977260A (en) * 2012-07-20 2013-03-20 苏州大学 Macromolecule bonding agent and preparation method thereof
FR3017616A1 (en) * 2014-02-20 2015-08-21 Herakles LOADING PROPERGOL, WITH MECHANICALLY REINFORCED LIEUR / PROPERGOL LINK AND PREPARATION
CN105481704A (en) * 2016-01-12 2016-04-13 西安近代化学研究所 Method for synthesis and purification of bonding agent N-propargyl diethanol amine
CN107628969A (en) * 2017-10-21 2018-01-26 湖北三江航天江河化工科技有限公司 A kind of amide-type aid and its synthetic method for composite solidpropellant

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102007029644A1 (en) * 2007-06-26 2009-01-08 Henkel Ag & Co. Kgaa One-component, hot-curing reactive composition
CN101113123A (en) * 2007-07-16 2008-01-30 上海东方久乐汽车安全气囊有限公司 Multiple micro-porous gas production charge column and method for making same
US20130048163A1 (en) * 2011-08-31 2013-02-28 Alliant Techsystems Inc. Propellant compositions including stabilized red phosphorus, a method of forming same, and an ordnance element including the same
CN102977260A (en) * 2012-07-20 2013-03-20 苏州大学 Macromolecule bonding agent and preparation method thereof
FR3017616A1 (en) * 2014-02-20 2015-08-21 Herakles LOADING PROPERGOL, WITH MECHANICALLY REINFORCED LIEUR / PROPERGOL LINK AND PREPARATION
CN105481704A (en) * 2016-01-12 2016-04-13 西安近代化学研究所 Method for synthesis and purification of bonding agent N-propargyl diethanol amine
CN107628969A (en) * 2017-10-21 2018-01-26 湖北三江航天江河化工科技有限公司 A kind of amide-type aid and its synthetic method for composite solidpropellant

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