CN101891565A - Preparation method of emulsifier for electric blasting - Google Patents

Preparation method of emulsifier for electric blasting Download PDF

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Publication number
CN101891565A
CN101891565A CN2010102303956A CN201010230395A CN101891565A CN 101891565 A CN101891565 A CN 101891565A CN 2010102303956 A CN2010102303956 A CN 2010102303956A CN 201010230395 A CN201010230395 A CN 201010230395A CN 101891565 A CN101891565 A CN 101891565A
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reactor
stop
vacuum pump
stir
open
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CN2010102303956A
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Inventor
钱泽文
史景忠
李广辉
刘品正
宋维功
夏振岭
范宝石
王敏
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Pingdingshan Power Supply Co of State Grid Henan Electric Power Co Ltd
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Pingdingshan Power Supply Co of State Grid Henan Electric Power Co Ltd
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Publication of CN101891565A publication Critical patent/CN101891565A/en
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Abstract

The invention discloses a preparation method of an emulsifier for electric blasting. The method comprises the following steps of: stirring sorbitol, adding an aqueous phosphorous acid solution and heating the mixture to 115-150 DEG C; adding 500-530kg of oleic acid into a reactor, and stirring the mixture; slowly adding an aqueous sodium hydroxide solution into the reactor and quickly heating the reactor to 210 DEG C; maintaining the temperature of the reactor for 3 hours; sampling, stirring the mixture and assaying the acid value, the specific viscosity and a measured hydroxyl value; when the vacuum pressure reaches 0.06-0.11MPa, filtering the mixture in vacuum, standing for 10-12 hours and cooling; and uniformly mixing lecithin and T-152 emulsifier. In the method, mixed hydramine in a proper proportion is selected to react with carboxylic acid, thereby the steric effect in the reaction is reduced, and the emulsifier can obtain larger hydrophilic groups; and moreover, the hydrophilic groups have stable property so that the property stability of powdered emulsion explosives in the processes of production and storage is improved.

Description

The preparation method of emulsifier for electric blasting
Technical field
The invention belongs to the preparation method of powdery emulsifying explosive emulsification reagent technical field, particularly a kind of emulsifier for electric blasting.
Background technology
Powdery emulsifying explosive is a kind of civil blast explosive, and it is to be that disperse phase, combustible agent oil phase are external phase by aqueous oxidizing agent solution, is prepared into the emulsion matrix of water-in-oil-type, the powder type explosive that uses drying process with atomizing to make then by the effect of emulsifying agent.It is a kind ofly both to have possessed that the emulsion explosive blast performance is good, component does not contain TNT, has the characteristics of certain water repelling property, possesses the powdery ammonium ladder detonator shelf-stable again, uses the novel emulsion explosive of advantage such as more flexible.
ZL96100379.0 proposes a kind of emulsifying agent that is used for emulsion explosive and preparation method thereof, carry out esterification with poly-hydrocarbon carboxylic acids or acid anhydrides with polyvalent alcohol under the effect of catalyzer, it is good and be suitable for preparing the water-in-oil-type macromolecule emulsifier of high storage stability energy emulsion explosive to obtain a kind of each form a social stratum performance.This emulsifying agent molecular structure is that its hydrophilic group at the emulsion explosive technological design is the ester class formation, does not contain and the jealous woman amine groups, compares with succimide, emulsifying property improves a lot, but the emulsifying base of preparation is softer, becomes the powder difficulty, therefore is unsuitable for producing powdery emulsifying explosive.Relate to a kind of emulsifying agent in the disclosed water-base drilling fluid of WO96/40835, comprised the reaction product of a kind of poly-hydrocarbon carboxylic acids or acid anhydrides and hydramine, but it at be drilling fluid, can not be most appropriate to powdery emulsifying explosive.
Summary of the invention
The invention provides a kind of easy emulsification, emulsifying stability is good, and is beneficial to the preparation method that explosive is sprayed into the emulsifying agent that the powdery emulsifying explosive of powder uses.
A kind of preparation method of emulsifier for electric blasting may further comprise the steps:
A), start vacuum pump and in reactor, extract ready sorbyl alcohol 250Kg~280Kg, stop vacuum pump, open and stir, add the phosphorous acid aqueous solution of 1.5Kg~2.5Kg, the startup hot oil pump makes the reactor rapid heating;
B), the question response temperature in the kettle picks up counting when rising to 90 ℃~115 ℃, slowly rises with per hour 10 ℃~15 ℃ speed, rose between 115 ℃~150 ℃ through about 3 hours;
C), stop to stir, open vacuum pump, 500Kg~530Kg oleic acid is added in the reactor, stop vacuum pump, open and stir, the aqueous sodium hydroxide solution of 3.2Kg~5.4Kg is slowly added in the reactor, be rapidly heated;
D), pick up counting during question response still temperature to 180 ℃~200 ℃, insulation is 3 hours when rising to 210 ℃;
E), stop stirring, sampling, unlatching stirring chemical examination acid number, specific viscosity, survey hydroxyl value;
F), when opening vacuum pump and making vacuum pressure in the reactor reach 0.06Mpa~0.11Mpa, behind the vacuum reaction about in half an hour, stop to stir, open the vacuum punishment in advance to leaving standstill;
G), through cooling in 10~12 hours, leave standstill the back earlier with after the sugared slag emptying, discharging then; H), the Yelkin TTS of remix 400Kg~450Kg and 20Kg~35Kg T-152 type emulsifying agent mixing gets final product.
As of the present invention a kind of preferred, the preparation method of emulsifier for electric blasting may further comprise the steps:
A), start vacuum pump and in reactor, extract ready sorbyl alcohol 265Kg, stop vacuum pump, open and stir, add the phosphorous acid aqueous solution of 2Kg, the startup hot oil pump makes the reactor rapid heating;
B), the question response temperature in the kettle picks up counting when rising to 105 ℃, slowly rises with 12 ℃ speed per hour, rose between 115 ℃~150 ℃ through about 3 hours;
C), stop to stir, open vacuum pump, 510Kg oleic acid is added in the reactor, stop vacuum pump, open and stir, the aqueous sodium hydroxide solution of 4.4Kg is slowly added in the reactor, be rapidly heated;
D), pick up counting during question response still temperature to 180 ℃, insulation is 3 hours when rising to 210 ℃;
E), stop stirring, sampling, unlatching stirring chemical examination acid number, specific viscosity, survey hydroxyl value;
F), when opening vacuum pump and making vacuum pressure in the reactor reach 0.08Mpa, behind the vacuum reaction about in half an hour, stop to stir, open the vacuum punishment in advance to leaving standstill;
G), through cooling in 11 hours, leave standstill the back earlier with after the sugared slag emptying, discharging then;
H), the Yelkin TTS of remix 420Kg and 28KgT-152 type emulsifying agent mixing get final product.
Because powdery emulsifying explosive of the present invention has been selected the mixing hydramine and the carboxylic acid reaction of suitable proportion for use with the preparation method of emulsifying agent, steric effect in the reaction reduces to know clearly, can make emulsifying agent obtain bigger hydrophilic radical, and this hydrophilic radical stable in properties, the stability of raising powdery emulsifying explosive performance in production and storage process.Add another kind of T152 type emulsifying agent in addition, not only improved emulsifying property, and the continuous compactness of emulsifying film is increased, thereby further improve the package stability of explosive.Use the emulsifying agent of the inventive method preparation, can reduce the emulsifying agent consumption, so the production security of the explosive made from present method is good.The preparation method of emulsion of the present invention is simple, and raw material is easy to get, and need not reaction process is carried out precision control.
Embodiment
Embodiment 1:
A kind of preparation method of emulsifier for electric blasting may further comprise the steps:
A), start vacuum pump and in reactor, extract ready sorbyl alcohol 250Kg, stop vacuum pump, open and stir, add the phosphorous acid aqueous solution of 1.5Kg, the startup hot oil pump makes the reactor rapid heating;
B), the question response temperature in the kettle picks up counting when rising to 90 ℃, slowly rises with 10 ℃ speed per hour, rises to 116 ℃ through about 3 hours;
C), stop to stir, open vacuum pump, 500Kg oleic acid is added in the reactor, stop vacuum pump, open and stir, the aqueous sodium hydroxide solution of 3.2Kg is slowly added in the reactor, be rapidly heated;
D), pick up counting during question response still temperature to 180 ℃, insulation is 3 hours when rising to 210 ℃;
E), stop stirring, sampling, unlatching stirring chemical examination acid number, specific viscosity, survey hydroxyl value;
F), when opening vacuum pump and making vacuum pressure in the reactor reach 0.06Mpa, behind the vacuum reaction about in half an hour, stop to stir, open the vacuum punishment in advance to leaving standstill;
G), through cooling in 10 hours, leave standstill the back earlier with after the sugared slag emptying, discharging then; H), the Yelkin TTS of remix 400Kg and 20Kg T-152 type emulsifying agent mixing get final product.
Embodiment 2:
A kind of preparation method of emulsifier for electric blasting may further comprise the steps:
A), start vacuum pump and in reactor, extract ready sorbyl alcohol 280Kg, stop vacuum pump, open and stir, add the phosphorous acid aqueous solution of 2.5Kg, the startup hot oil pump makes the reactor rapid heating;
B), the question response temperature in the kettle picks up counting when rising to 115 ℃, slowly rises with 15 ℃ speed per hour, rose between 150 ℃ through about 3 hours;
C), stop to stir, open vacuum pump, 530Kg oleic acid is added in the reactor, stop vacuum pump, open and stir, the aqueous sodium hydroxide solution of 5.4Kg is slowly added in the reactor, be rapidly heated;
D), pick up counting during question response still temperature to 200 ℃, insulation is 3 hours when rising to 210 ℃;
E), stop stirring, sampling, unlatching stirring chemical examination acid number, specific viscosity, survey hydroxyl value;
F), when opening vacuum pump and making vacuum pressure in the reactor reach 0.11Mpa, behind the vacuum reaction about in half an hour, stop to stir, open the vacuum punishment in advance to leaving standstill;
G), through cooling in 12 hours, leave standstill the back earlier with after the sugared slag emptying, discharging then;
H), the Yelkin TTS of remix 450Kg and 35Kg T-152 type emulsifying agent mixing get final product.
Embodiment 3:
A kind of preparation method of emulsifier for electric blasting may further comprise the steps:
A), start vacuum pump and in reactor, extract ready sorbyl alcohol 265Kg, stop vacuum pump, open and stir, add the phosphorous acid aqueous solution of 2Kg, the startup hot oil pump makes the reactor rapid heating;
B), the question response temperature in the kettle picks up counting when rising to 105 ℃, slowly rises with 12 ℃ speed per hour, rose between 115 ℃~150 ℃ through about 3 hours;
C), stop to stir, open vacuum pump, 510Kg oleic acid is added in the reactor, stop vacuum pump, open and stir, the aqueous sodium hydroxide solution of 4.4Kg is slowly added in the reactor, be rapidly heated;
D), pick up counting during question response still temperature to 180 ℃, insulation is 3 hours when rising to 210 ℃;
E), stop stirring, sampling, unlatching stirring chemical examination acid number, specific viscosity, survey hydroxyl value;
F), when opening vacuum pump and making vacuum pressure in the reactor reach 0.08Mpa, behind the vacuum reaction about in half an hour, stop to stir, open the vacuum punishment in advance to leaving standstill;
G), through cooling in 11 hours, leave standstill the back earlier with after the sugared slag emptying, discharging then;
H), the Yelkin TTS of remix 420Kg and 28Kg T-152 type emulsifying agent mixing get final product.Comparative example 1 (ZL96100379.0 example 1)
With the 200Kg saponification value is polybutene base maleic anhydride 25Kg glycol ether and the mixing of 3Kg30%NaOH solution of 70mgKOH/g, adds the 0.2Kg silicon oil foam killer.Heating also is evacuated, and reaction finished in 3 hours under 200 ℃-0.1Mpa.
Comparative example 2:
According to embodiment 2, but do not add Yelkin TTS and T-152 type emulsifying agent at last, other are identical with embodiment 2.
Table 1:
Figure BSA00000195948100051
The emulsifying agent of embodiment of the invention preparation, comparative example emulsifying agent pass through to change emulsification still mixing speed with T-154 and T-155, under different emulsion strengths, carry out the emulsion test of powdery emulsifying explosive, other conditions constant (as shown in table 2), the result shows that the emulsifying agent that the present invention prepares can form emulsification system when hanging down emulsion strength, can reduce emulsion strength when promptly the emulsifying agent for preparing with the present invention prepares powdery emulsifying explosive, make the emulsification spare part mild, thereby significantly improve the production security of powdery emulsifying explosive.
The one-tenth breast speed of table 2 emulsifying agent under different emulsion strengths
Figure BSA00000195948100061
(annotate: T-152, T-154, T-155 type emulsifying agent are additive factory of Jinzhou petro-chemical corporation and produce, and a large amount of supplies are all arranged on the market, are to be reacted with triethylene tetramine or tetraethylene pentamine by the polyisobutenyl maleic anhydride to make.)
Because powdery emulsifying explosive of the present invention has been selected the mixing hydramine and the carboxylic acid reaction of suitable proportion for use with the preparation method of emulsifying agent, steric effect in the reaction reduces to know clearly, can make emulsifying agent obtain bigger hydrophilic radical, and this hydrophilic radical stable in properties, the stability of raising powdery emulsifying explosive performance in production and storage process.Add another kind of T-152 type emulsifying agent in addition, not only improved emulsifying property, and the continuous compactness of emulsifying film is increased, thereby further improve the package stability of explosive.Use the emulsifying agent of the inventive method preparation, can reduce the emulsifying agent consumption, so the production security of the explosive made from present method is good.The preparation method of emulsion of the present invention is simple, and raw material is easy to get, and need not reaction process is carried out precision control.

Claims (2)

1. the preparation method of an emulsifier for electric blasting is characterized in that, it may further comprise the steps:
A), start vacuum pump and in reactor, extract ready sorbyl alcohol 250Kg~280Kg, stop vacuum pump, open and stir, add the phosphorous acid aqueous solution of 1.5Kg~2.5Kg, the startup hot oil pump makes the reactor rapid heating;
B), the question response temperature in the kettle picks up counting when rising to 90 ℃~115 ℃, slowly rises with per hour 10 ℃~15 ℃ speed, rose between 115 ℃~150 ℃ through about 3 hours;
C), stop to stir, open vacuum pump, 500Kg~530Kg oleic acid is added in the reactor, stop vacuum pump, open and stir, the aqueous sodium hydroxide solution of 3.2Kg~5.4Kg is slowly added in the reactor, be rapidly heated;
D), pick up counting during question response still temperature to 180 ℃~200 ℃, insulation is 3 hours when rising to 210 ℃;
E), stop stirring, sampling, unlatching stirring chemical examination acid number, specific viscosity, survey hydroxyl value;
F), when opening vacuum pump and making vacuum pressure in the reactor reach 0.06Mpa~0.11Mpa, behind the vacuum reaction about in half an hour, stop to stir, open the vacuum punishment in advance to leaving standstill;
G), through cooling in 10~12 hours, leave standstill the back earlier with after the sugared slag emptying, discharging then;
H), the Yelkin TTS of remix 400Kg~450Kg and 20Kg~35Kg T-152 type emulsifying agent mixing gets final product.
2. ammonium nitrate modifier for electric blasting as claimed in claim 1, it is characterized in that: it may further comprise the steps:
A), start vacuum pump and in reactor, extract ready sorbyl alcohol 265Kg, stop vacuum pump, open and stir, add the phosphorous acid aqueous solution of 2Kg, the startup hot oil pump makes the reactor rapid heating;
B), the question response temperature in the kettle picks up counting when rising to 105 ℃, slowly rises with 12 ℃ speed per hour, rose between 115 ℃~150 ℃ through about 3 hours;
C), stop to stir, open vacuum pump, 510Kg oleic acid is added in the reactor, stop vacuum pump, open and stir, the aqueous sodium hydroxide solution of 4.4Kg is slowly added in the reactor, be rapidly heated;
D), pick up counting during question response still temperature to 180 ℃, insulation is 3 hours when rising to 210 ℃;
E), stop stirring, sampling, unlatching stirring chemical examination acid number, specific viscosity, survey hydroxyl value;
F), when opening vacuum pump and making vacuum pressure in the reactor reach 0.08Mpa, behind the vacuum reaction about in half an hour, stop to stir, open the vacuum punishment in advance to leaving standstill;
G), through cooling in 11 hours, leave standstill the back earlier with after the sugared slag emptying, discharging then;
H), the Yelkin TTS of remix 420Kg and 28KgT-152 type emulsifying agent mixing get final product.
CN2010102303956A 2010-07-20 2010-07-20 Preparation method of emulsifier for electric blasting Pending CN101891565A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106083497A (en) * 2016-06-23 2016-11-09 湖北同石油化工有限公司 A kind of LZ2735 emulsifying agent and preparation method thereof
CN112898621A (en) * 2021-03-16 2021-06-04 青岛瑞诺化工有限公司 Emulsifier, preparation method thereof and application thereof in latex foaming product

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106083497A (en) * 2016-06-23 2016-11-09 湖北同石油化工有限公司 A kind of LZ2735 emulsifying agent and preparation method thereof
CN112898621A (en) * 2021-03-16 2021-06-04 青岛瑞诺化工有限公司 Emulsifier, preparation method thereof and application thereof in latex foaming product

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