CN101152993B - Emulsifying agent for emulsification blasting agent mixing vehicle and synthesizing method thereof - Google Patents
Emulsifying agent for emulsification blasting agent mixing vehicle and synthesizing method thereof Download PDFInfo
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- CN101152993B CN101152993B CN2006100479543A CN200610047954A CN101152993B CN 101152993 B CN101152993 B CN 101152993B CN 2006100479543 A CN2006100479543 A CN 2006100479543A CN 200610047954 A CN200610047954 A CN 200610047954A CN 101152993 B CN101152993 B CN 101152993B
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Abstract
The present invention provides an emulsifier for emulsified explosive mixture vehicle, comprising the components as formula (I)-(IV). The content of each component is as follows: (I) is equal to 30 -70 wt%, (II) is equal to 10 -50 wt%, (III) is equal to 10 - 40 wt%, and (IV) is equal to 10 - 20 wt%. The synthesis method of the emulsifier comprises the following steps: mixing 20 - 40 wt% of hydroxy-terminated polyoxyethylene, 20 - 40 wt% of polyisobutylene anhydride, 0.3 -1.2 wt% of NaOH or KOH aqueous solution (with concentration of 30 - 60 wt%); heating and vacuumizing; carrying out esterification reaction for 3 to 8 hours at a temperature between 150 DEG C to 300 DEG C and under pressure of minus 0.02MPa to minus 0.08MPa; cooling to 60-120 DEG C, adding 20 - 50 wt% of alkyl sulfonate aqueous solution (with concentration of 30 - 70 wt%); keeping the temperature for 1 to 3hours under atmospheric pressure. The emulsifier has the characteristics of low cost, good hydrophilicity, easy emulsification and so on; a composite three-dimensional mesh interface membrane can be formed in the emulsification process; the strength and thickness of emulsified film are increased; the emulsion effects and emulsion stability are improved; the prepared latex matrix has good stability of storage; the emulsified explosives has good water resistance, no detonator sensitivity and good security.
Description
Technical field
The present invention relates to the emulsifying agent technology, in particular for the emulsifying agent and the synthetic method thereof of emulsification blasting agent mixing vehicle.
Background technology
Emulsification blasting agent mixing vehicle is the scene of ore deposit explosion in the open, carries out continuous emulsification and sensitization process for processing emulsion explosive on emulsification blasting agent mixing vehicle, and be delivered directly to that transporting something containerized in the big gun hole is defeated, preparation, powder charge be in the automaticmachines equipment of one.The emulsion explosive of preparation is water-in-oil-type (w/o), no cap-sensitivity, and it is good to have a security, and preparation technology is simple, characteristics such as detonation property excellence.Emulsion explosive mainly is made up of aqueous inorganic oxidizer salt solution, oil phase material and emulsifying agent.Effect by emulsifying agent make be lower than the 10wt% oil phase material as external phase with the emulsification under the effect of mechanical dispersion power of the aqueous inorganic oxidizer salt solution more than the 90wt%, form the emulsion matrix of water-in-oil-type (w/o).Because emulsion matrix is non-thermodynamic stable system, the disperse phase that is dispersed in the external phase exists with the fine droplet form, very easily gathering, breakdown of emulsion.Emulsion matrix stability depends on the interface film strength, and the interfacial film thickness of the structure of interface film strength and emulsifying agent and formation is closely related.Therefore, emulsifying agent is the major cause that influences emulsion matrix stability.
At present, the emulsifying agent of using at emulsification blasting agent mixing vehicle is mainly Sp-80.It is that emulsifying agent prepares emulsion explosive that patent EP01429 proposes with Sp-80, and the compactness of the emulsifying film of its formation and film toughness are all very poor, so stability is very low.Played certain effect for improving stability adding emulsion stabilizer, but effect is still undesirable.The preparation that macromolecule emulsifier is applied to emulsion explosive was arranged in recent years, propose with polymer alkyl substituted carboxylic acid and polyamine compounds prepared in reaction succimide family macromolecule emulsifying agent as patent USP4708753, USP4828633 and GB2216128, though improved emulsification film strength and snappiness, but its number average relative molecular weight is bigger, and hydrophilic radical is few, so emulsifying power is low, the shearing resistance height that emulsification is required.This class emulsifying agent high temperature easily decomposes generation ammonia and carbonic acid gas, and the emulsion matrix of preparation has certain detonation susceptibility, is not suitable for emulsification blasting agent mixing vehicle.The polyisobutene series emulsifier viscosity of domestic production is big, does not meet the emulsification blasting agent mixing vehicle requirement, so seldom be applied to the blasting agent mixing vehicle industrial production.
Summary of the invention
The object of the present invention is to provide a kind of easy emulsification, good stability, cheap, and be applicable to composite high-molecular emulsifying agent that emulsification blasting agent mixing vehicle uses and preparation method thereof.
The moiety that the present invention is used for the emulsifying agent of emulsification blasting agent mixing vehicle is:
(III)R
3-SO
3Na
(IV) water
In the formula: n=5～30; R
1Be C
2～C
12Alkyl; R
2Be C
5～C
80Alkyl; R
3Be C
8～C
20Alkyl;
Each components contents (by weight percentage) is:
(I)：30％～70％；(II)：10％～50％；(III)：10％～40％；(IV)：10％～20％。
The synthetic method of emulsifying agent that the present invention is used for emulsification blasting agent mixing vehicle is as follows: will (by weight percentage) terminal hydroxy group Soxylat A 25-7 20%～40%, polyisobutene acid anhydrides or polyisobutene carboxylic acid 20%～40% and (concentration weight percent 30%～60%) NaOH or the KOH aqueous solution 0.3%～1.2% mix, heating vacuumizes, at 150～300 ℃,-0.02～-the 0.08MPa condition under esterification after 3～8 hours, be cooled to 60～120 ℃, add (concentration weight percent 30%～70%) alkylsulphonic acid sodium water solution 20%～50%, normal pressure constant temperature is 1～3 hour again, and reaction finishes.
R in the reactant of the present invention
1Be preferably C
2～C
6Alkyl; R
2Be preferably C
5～C
30Alkyl; R
3Be preferably C
12～C
18Alkyl.
The end group of reactant terminal hydroxy group Soxylat A 25-7 of the present invention is preferably the both-end hydroxyl, and the polymerization degree n of terminal hydroxy group Soxylat A 25-7 preferably is controlled in 5～10 scopes.
Reactant polyisobutene acid anhydrides of the present invention or polyisobutene carboxylic acid can be polyisobutene maleic anhydride or polyisobutene fumaric acid.
The esterification reaction temperature of reactant of the present invention is preferably 150～200 ℃.
The present invention is introduced the hydrophilic radical of longer carbon oxygen chain by the composite high-molecular emulsifying agent of terminal hydroxy group Soxylat A 25-7, polyisobutene acid anhydrides and alkylsulfonate preparation, adopted compounded technology, solved that single macromolecule emulsifier viscosity is too high, the insufficient shortcoming of wetting ability, had characteristics such as cost is low, easy emulsification; In emulsion process, can form compounding solid netted interfacial film, increase emulsification film strength and thickness, improve emulsifying effectiveness and emulsifying stability; The emulsion matrix storage stability of preparation is good, and emulsion explosive water resisting property is good, no cap-sensitivity, and security is good.
Embodiment 1
With 80.1g polyisobutene maleic anhydride (number average relative molecular mass=1309), 1.5g concentration is the KOH aqueous solution and the 53.2g HOCH of 50wt%
2CH
2O (CH
2-CH
2O)
10CH
2CH
2OH mixes, and heating vacuumizes, 180 ℃ ,-the 0.07MPa condition under esterification after 4 hours, be cooled to 105 ℃, adding 80.2g concentration is the sodium dodecyl sulfate aqueous solution of 40wt%, normal pressure constant temperature is 1 hour again, reaction finishes.Product kinematic viscosity (100 ℃): 2452.8mm
2/ s; Water-content: 19.1wt%; Acid number (mg KOH/g): 22.5.
Embodiment
Embodiment 2
With 100.0g polyisobutene fumaric acid (number average relative molecular mass=986), concentration is KOH aqueous solution 3.2g and the 100.4g HOCH of 30wt%
2CH
2O (CH
2-CH
2O)
10CH
2CH
2OH mixes, and heating vacuumizes, 160 ℃ ,-the 0.08MPa condition under esterification after 5 hours, be cooled to 100 ℃, adding concentration is the sodium dodecyl sulfate aqueous solution 96.2g of 40wt%, normal pressure constant temperature is 1 hour again, reaction finishes.Product kinematic viscosity (100 ℃): 1618.5mm
2/ s; Water-content: 18.2wt%; Acid number (mg KOH/g): 25.3.
Embodiment 3
With 79.8g polyisobutene maleic anhydride (number average relative molecular mass=979), concentration is NaOH aqueous solution 1.6g and the 76.1g HO (CH of 40wt%
2)
3O (CH
2-CH
2O)
5(CH
2)
6OH stirs, 150 ℃ ,-the 0.08MPa condition under esterification after 6 hours, be cooled to 95 ℃,
Adding concentration is the Sodium dodecylbenzene sulfonate 142.9g of 30wt%, and normal pressure constant temperature is 1.5 hours again, and reaction finishes.Product kinematic viscosity (100 ℃): 1632.2mm
2/ s; Water-content: 18.1wt%; Acid number (mgKOH/g): 20.3.
Embodiment 4
KOH aqueous solution 1.7g and 68.3g HO (CH with 120.1g polyisobutene maleic anhydride (number average relative molecular mass=1123), concentration 40wt%
2)
3O (CH
2-CH
2O)
3(CH
2)
3OH stirs, 200 ℃ ,-the 0.06MPa condition under reaction after 4 hours, be cooled to 100 ℃, adding concentration is the sodium dodecyl sulfate aqueous solution 141.3g of 40wt%, normal pressure constant temperature is 1.5 hours again, reaction finishes.Product kinematic viscosity (100 ℃): 1721.2mm
2/ s; Water-content: 19.5wt%; Acid number (mg KOH/g): 24.8.
Embodiment 5
With 90.1g polyisobutene maleic anhydride (number average relative molecular mass=983.5), concentration 40wt%NaOH aqueous solution 1.5g and 58.0g HOCH
2CH
2O (CH
2-CH
2O)
8CH
2CH
2OH stirs, 200 ℃ ,-the 0.06MPa condition under reaction after 4 hours, be cooled to 105 ℃, adding concentration is 40Wt% sodium laurylsulfonate 111.1g, normal pressure constant temperature is 1 hour again, reaction finishes.Product kinematic viscosity (100 ℃): 2421.5mm
2/ s; Water-content: 18.7wt%; Acid number (mg KOH/g): 23.6.
Claims (6)
1. the synthetic method of an emulsifying agent, it is characterized in that terminal hydroxy group Soxylat A 25-7 20%～40%, polyisobutene acid anhydrides or polyisobutene carboxylic acid 20%～40% and (concentration weight percent 30%～60%) NaOH or 0.3%～1.2% mixing of the KOH aqueous solution by weight percentage, heating vacuumizes, 150～300 ℃ ,-0.02～-the 0.08MPa condition under esterification after 3～8 hours, be cooled to 60～120 ℃, add (concentration weight percent 30%～70%) alkylsulphonic acid salt brine solution 20%～50%, normal pressure constant temperature is 1～3 hour again, and reaction finishes.
2. the synthetic method of emulsifying agent according to claim 1, the esterification reaction temperature that it is characterized in that described reactant is 150～200 ℃.
3. the synthetic method of emulsifying agent according to claim 1, the end group that it is characterized in that described reactant terminal hydroxy group Soxylat A 25-7 is the both-end hydroxyl.
4. the synthetic method of emulsifying agent according to claim 1, the content weight percent that it is characterized in that described reactant alkylsulfonate is 10%～30%.
5. the synthetic method of emulsifying agent according to claim 1 is characterized in that described reactant polyisobutene acid anhydrides or polyisobutene carboxylic acid can be polyisobutene maleic anhydride or polyisobutene fumaric acid.
6. the synthetic method of emulsifying agent according to claim 1 is characterized in that described reactant alkylsulfonate can be sodium salt or sylvite.
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|---|---|---|---|
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| CN101152993B true CN101152993B (en) | 2011-08-17 |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102584502B (en) * | 2012-01-12 | 2014-06-04 | 南京理工大学 | Method for preparing macromolecular emulsifying agent |
| CN102675004B (en) * | 2012-05-15 | 2014-10-08 | 鞍钢集团矿业设计研究院 | Composite oil phase for bulk waterproof emulsion explosive and preparation method thereof |
| CN105348416B (en) * | 2015-11-03 | 2017-12-08 | 葛洲坝易普力股份有限公司 | Emulsion macromolecule emulsifier and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1156137A (en) * | 1995-11-08 | 1997-08-06 | 帝国化学工业(加拿大)有限公司 | Emulgent for explosive composition |
| CN1158833A (en) * | 1996-01-17 | 1997-09-10 | 中国石油化工总公司 | Emulsifier for emulsified explosive and its preparation process |
| CN1362389A (en) * | 2001-01-05 | 2002-08-07 | 中国石油化工股份有限公司 | Emulsified explosive |
| WO2003053884A1 (en) * | 2001-12-20 | 2003-07-03 | Nippon Kayaku Kabushiki Kaisha | Explosive |
| CN1609079A (en) * | 2003-10-24 | 2005-04-27 | 中国石油化工股份有限公司 | Emulsifier for powdered emulsified explosive and its prepn process |
-
2006
- 2006-09-29 CN CN2006100479543A patent/CN101152993B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1156137A (en) * | 1995-11-08 | 1997-08-06 | 帝国化学工业(加拿大)有限公司 | Emulgent for explosive composition |
| CN1158833A (en) * | 1996-01-17 | 1997-09-10 | 中国石油化工总公司 | Emulsifier for emulsified explosive and its preparation process |
| CN1362389A (en) * | 2001-01-05 | 2002-08-07 | 中国石油化工股份有限公司 | Emulsified explosive |
| WO2003053884A1 (en) * | 2001-12-20 | 2003-07-03 | Nippon Kayaku Kabushiki Kaisha | Explosive |
| CN1609079A (en) * | 2003-10-24 | 2005-04-27 | 中国石油化工股份有限公司 | Emulsifier for powdered emulsified explosive and its prepn process |
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Address after: 114001 Anshan District, Liaoning, No. 219 Road, No. 39, Tiedong Patentee after: Anshan Iron and Steel Group Mining Co., Ltd. Address before: 114001 Anshan District, Liaoning, No. 219 Road, No. 39, Tiedong Patentee before: Angang Group Mine Company |