CN110862471A - Method for synthesizing polyisobutylene succinic acid alcohol ester high-molecular emulsifier for emulsion explosive - Google Patents

Method for synthesizing polyisobutylene succinic acid alcohol ester high-molecular emulsifier for emulsion explosive Download PDF

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CN110862471A
CN110862471A CN201911083567.9A CN201911083567A CN110862471A CN 110862471 A CN110862471 A CN 110862471A CN 201911083567 A CN201911083567 A CN 201911083567A CN 110862471 A CN110862471 A CN 110862471A
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polyisobutylene succinic
succinic acid
polyisobutylene
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黄正华
李艺
吕鹏飞
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GEZHOUBA YIPULI HUBEI CHANGTAI CIVIL EXPLOSIVE CO Ltd
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Abstract

A synthetic method of a polyisobutene succinic acid alcohol ester high molecular emulsifier for emulsion explosives comprises the following steps: 1) the first step is that polyisobutylene and maleic anhydride are subjected to thermal addition reaction to prepare polyisobutylene succinic anhydride; carrying out alkylation reaction on polyisobutylene and maleic anhydride at 160-220 ℃ for 4-7 hours by a thermal heating method to generate a polyisobutylene succinic anhydride crude product; 2) and (3) carrying out esterification reaction on the purified polyisobutene succinic anhydride, toluene and glycerol serving as solvents at 100-150 ℃ under the action of sulfuryl chloride, wherein the reaction time is 3-8 hours, and thus polyisobutene succinic acid alcohol ester is generated. The invention has the advantages that the liquid chlorine pollution source is eradicated from the process route, thereby reducing a chlorine system and a hydrogen chloride absorption system for producing the alkene anhydride by the chlorination process. When the method is adopted for production, the polyisobutylene succinic acid alcohol ester high molecular emulsifier with excellent quality can be continuously and rapidly produced, and the storage stability of the emulsion explosive is obviously improved.

Description

Method for synthesizing polyisobutylene succinic acid alcohol ester high-molecular emulsifier for emulsion explosive
Technical Field
The invention relates to a method for synthesizing an emulsifier, in particular to a method for synthesizing a polyisobutylene succinic acid alcohol ester high molecular emulsifier for emulsion explosives.
Background
Since the self-emulsifying explosive as a novel industrial water-resistant explosive became available in the end of the 60 s, the self-emulsifying explosive rapidly gained the attention of the industrial explosive world and competitively researched and popularized. However, there is a disadvantage that the development thereof is largely limited, i.e., the insufficient storage stability, and the main problem in the study of emulsion explosives is how to improve the stability of emulsion explosives.
The emulsifier is used as the most key component of the emulsion explosive, and the quality of the emulsifying capacity directly influences the stability of the emulsion explosive, so that the stability of the emulsion explosive must be changed fundamentally from the emulsifier to improve the stability of the emulsion explosive, which is the key point for solving the problem of insufficient stability of the emulsion explosive.
The emulsifier commonly used in the industry at present is Span80, which is easy to emulsify and has good shear stability, but the storage life of the emulsion explosive prepared by using Span80 as the emulsifier is short; the emulsion explosive prepared by the agent T has long storage period, but the emulsifying power is not good; the compound of Span80 and T agent improves the emulsification and storage stability of the emulsion explosive, but the simple physical mixing can not completely achieve the expected target to some extent, the purposes of reducing the shearing linear velocity and improving the storage period during emulsification can not be really realized, and the compound proportion is not easy to determine.
Therefore, the emulsifier which has good emulsibility, long storage time of the prepared emulsion explosive and is economical and applicable is developed and is very important for the development of the emulsion explosive. The novel emulsifier is synthesized to improve the stability of the emulsion explosive in the production and storage processes, so that the synthesized emulsifier has the characteristics of good emulsifying capacity, moderate matrix viscosity, high emulsion forming speed and the like, and the novel emulsifier is favorable for the production and storage of the emulsion explosive. The synthesized polyisobutene succinic acid alcohol ester high molecular emulsifier can be applied to emulsion explosives and can also be used as a lubricating oil additive, so that insoluble substances generated in the use process of fuel oil are kept suspended, particle agglomeration is prevented, and the viscosity increase of the fuel oil in the use process is inhibited.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for synthesizing a polyisobutene succinic acid alcohol ester high-molecular emulsifier for emulsion explosives, which can solve the problem of producing the high-molecular emulsifier by a chlorination method, and can continuously and quickly produce the polyisobutene succinic acid alcohol ester high-molecular emulsifier with excellent quality by adopting a new method for production.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows: a synthetic method of a polyisobutene succinic acid alcohol ester high molecular emulsifier for emulsion explosives comprises the following steps:
1) the first step is that polyisobutylene and maleic anhydride are subjected to thermal addition reaction to prepare polyisobutylene succinic anhydride;
carrying out alkylation reaction on polyisobutylene and maleic anhydride at 160-220 ℃ for 4-7 hours by a thermal heating method to generate a crude polyisobutylene succinic anhydride product, adding a proper amount of n-hexane to dissolve the product after the reaction is finished, and carrying out filtration, vacuum pumping, leaching and other processes to obtain pure polyisobutylene succinic anhydride (PIBSA);
2) and (2) carrying out esterification reaction on the purified polyisobutylene succinic anhydride (PIBSA) and solvents of toluene and glycerol under the action of sulfuryl chloride at the temperature of 100-150 ℃, wherein the reaction time is 3-8 hours, and generating polyisobutylene succinic acid alcohol ester which is a polyisobutylene succinic acid alcohol ester high-molecular emulsifier primary product for the emulsion explosive.
Preferably, the synthesis method of the polyisobutylene succinic acid ester high molecular emulsifier for the emulsion explosive further comprises the following steps:
adding saturated salt water into the primary product of the polyisobutylene succinic acid alcohol ester high molecular emulsifier for the emulsion explosive, removing unreacted glycerol, evaporating the obtained solution, and performing filtering separation and HLB value adjustment to obtain the finished product of the polyisobutylene succinic acid alcohol ester high molecular emulsifier for the emulsion explosive.
Preferably, in step 1), the polyisobutylene is high-activity polyisobutylene (with a number average molecular weight of 600).
Preferably, in the step 1), the polyisobutylene and the maleic anhydride are subjected to a heat heating method under the protection of nitrogen to produce high-content polyisobutylene succinic anhydride.
Preferably, in the step 2), the adding amount of sulfuryl chloride is 0.05 to 0.15 percent of the total mass.
Preferably, in the step 2), the mass of the polyisobutylene succinic anhydride is 200 to 500 percent of the mass of the glycerol.
Preferably, the mass of the saturated salt water is 0.04-0.06% of the mass of the primary product of the polyisobutylene succinic acid alcohol ester high-molecular emulsifier for the emulsion explosive.
Preferably, the HLB value is 3 to 6.
The invention adopts a thermal addition method for production, namely polyisobutylene succinic anhydride (PIBSA) and a certain amount of solvent toluene and glycerol are esterified and synthesized into a polyisobutylene succinic acid alcohol ester high molecular emulsifier primary finished product for emulsion explosives under the action of a sulfuryl chloride catalyst, and according to the synthesis process requirements: (1) the measurement of each raw material must be accurate, and the ratio can only be finely adjusted according to the quality difference of different batches of raw materials. (2) Purification is also required, namely: after the reaction is finished, adding a proper amount of n-hexane to dissolve the product, and carrying out processes such as filtering, vacuumizing, leaching and the like to obtain the pure polyisobutylene succinic anhydride (PIBSA).
(3) The temperature of the alkylation reaction is critical. This is because the alkylation reaction requires a large activation energy and is promoted by increasing the temperature, but the alkylation reaction is accompanied by side reactions, i.e., the self-polymerization of maleic anhydride and the degradation of polyisobutylene. When the temperature is not high, the side reaction is not obvious, and because the raw materials are excessive, the alkylation reaction rate is accelerated along with the rise of the temperature, the acid value of the product is gradually increased, but when the reaction temperature meets the requirement, the side reaction of the reaction is also intensified, a large amount of side reaction products are separated out, a plurality of coke-like objects appear, the color of the product is gradually deepened, the amount of the side reactant is large, and the acid value of the final product is low, so that the quality of the product is influenced.
(4) The alkylation reaction time is very critical. Since the longer the reaction time, the more thoroughly the two substances are mixed, the more complete the reaction and the acid value of the product increases. However, when the reaction time reaches a certain time, the reaction of the two substances is almost completed, the alkylation reaction is almost finished, and the acid value of the product does not obviously increase along with the increase of the time.
(5) The temperature and time of the esterification synthesis. In the esterification stage, the acid value and hydroxyl value of the product gradually decrease with the increase of the reaction temperature, because the esterification reaction is an endothermic reaction, the increase of the temperature is favorable for the reaction, and the water generated by the reaction is more easily evaporated with the increase of the temperature, and the reaction proceeds toward the positive direction, so that the acid value and hydroxyl value of the product gradually decrease.
As the reaction time is prolonged, the reaction of the intermediate PIBSA and the glycerol is more and more vigorous, the acid value and the hydroxyl value of the product are gradually reduced, and the acid value and the hydroxyl value of the product are not changed any more when a certain time is reached. The proper reaction temperature and time are required to be selected to ensure the normal reaction, so that the polyisobutylene succinic acid alcohol ester high molecular emulsifier with good quality is synthesized.
The invention provides a synthetic method of a polyisobutene succinic acid alcohol ester high molecular emulsifier for emulsion explosives, which adopts a thermal addition method for production, can realize automatic control production, continuously and quickly produce the polyisobutene succinic acid alcohol ester high molecular emulsifier with excellent quality, the produced emulsifier has the characteristics of good emulsifying capacity, moderate matrix viscosity, high emulsion forming speed and the like, and the production and storage performance of the explosives is stable. The emulsifier is especially suitable for the production process requirements of static emulsion and static sensitization emulsion explosives, the dosage of the emulsifier is small, the dispersibility and the storage stability are good, the storage stability can reach more than 6 months, and some can reach more than one year.
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The invention is further illustrated by the following examples in conjunction with the accompanying drawings:
FIG. 1 is a flow chart of the synthesis process of the present invention.
Detailed Description
Example 1
As shown in fig. 1, a synthesis method of polyisobutylene succinic acid alcohol ester polymer emulsifier for emulsion explosive comprises the following steps:
1) under the protection of nitrogen, 1000kg of high-activity polyisobutylene (with the number average molecular weight of 600) and 225kg of maleic anhydride are subjected to alkylation reaction at 170 ℃ by a thermal heating method for 3 hours to generate a crude product of the polyisobutylene succinic anhydride, a proper amount of normal hexane is added after the reaction is finished to dissolve the product, and processes such as filtering, vacuumizing and leaching are carried out to obtain pure polyisobutylene succinic anhydride (PIBSA);
2) carrying out esterification reaction on purified polyisobutene succinic anhydride (PIBSA) and a certain amount of solvent toluene and glycerol under the action of a high-efficiency catalyst sulfuryl chloride (the adding amount of the catalyst is 0.05-0.15 percent of the total mass) at 105 ℃, wherein the reaction time is 5 hours, and generating polyisobutene succinic acid alcohol ester, namely a polyisobutene succinic acid alcohol ester high-molecular emulsifier primary finished product for emulsion explosives;
3) adding a quantitative saturated salt solution into the polyisobutylene succinic acid alcohol ester high molecular emulsifier primary product for the emulsion explosive, removing unreacted glycerol, evaporating the obtained solution, and performing filtration separation and HLB value adjustment to obtain a finished polyisobutylene succinic acid alcohol ester high molecular emulsifier for the emulsion explosive.
In the step 2), the adopted catalyst is sulfuryl chloride, and the adding amount of the catalyst is 0.05-0.1% of the total mass. The mass of the polyisobutylene succinic anhydride (PIBSA) is 200-500% of that of the glycerol.
The product kinematic viscosity (100 ℃) of the prepared polyisobutene succinic acid alcohol ester polymer emulsifier finished product for the emulsion explosive is as follows: 202mm2(ii)/s, acid value: 35mgKOH/g, density (20 ℃ C.): 1112kg/m3The water content: 0.07%, minimum critical amount emulsification test: 0.60 percent, preparing the emulsion explosive according to the formula of the static emulsion and static sensitization emulsion explosive, observing the emulsion explosive by a polarizing microscope, and obviously crystallizing after storing for 5 months. The produced product is tested on a static emulsification and high-temperature static sensitization production line, and the production process, the sensitization process, the water-oil phase proportion and the like are not changed. After the test is carried out on the production line, the random sampling is carried out to detect the initial performance and carry out the natural storage performanceAnd (5) detecting, wherein the natural storage performance reaches 5 months. The results are as follows:
Figure BDA0002264686510000041
Figure BDA0002264686510000051
example 2
As shown in fig. 1, a synthesis method of polyisobutylene succinic acid alcohol ester polymer emulsifier for emulsion explosive comprises the following steps:
1) under the protection of nitrogen, 1000kg of high-activity polyisobutylene (with the number average molecular weight of 600) and 225kg of maleic anhydride are subjected to alkylation reaction at 140 ℃ by a thermal heating method for 6 hours to generate a crude product of the polyisobutylene succinic anhydride, a proper amount of normal hexane is added after the reaction is finished to dissolve the product, and processes such as filtering, vacuumizing and leaching are carried out to obtain the very pure polyisobutylene succinic anhydride (PIBSA);
2) carrying out esterification reaction on purified polyisobutene succinic anhydride (PIBSA) and a certain amount of solvent toluene and glycerol under the action of a high-efficiency catalyst sulfuryl chloride (the adding amount of the catalyst is 0.05-0.15 percent of the total mass) at 130 ℃, wherein the reaction time is 6 hours, and generating polyisobutene succinic alcohol ester, namely a polyisobutene succinic acid alcohol ester high-molecular emulsifier primary finished product for emulsion explosives;
3) adding a quantitative saturated salt solution into the polyisobutylene succinic acid alcohol ester high molecular emulsifier primary product for the emulsion explosive, removing unreacted glycerol, evaporating the obtained solution, and performing filtration separation and HLB value adjustment to obtain a finished polyisobutylene succinic acid alcohol ester high molecular emulsifier for the emulsion explosive.
In the step 2), the adopted catalyst is sulfuryl chloride, and the adding amount of the catalyst is 0.05-0.1% of the total mass. The mass of the polyisobutylene succinic anhydride (PIBSA) is 200-500% of that of the glycerol.
The product kinematic viscosity (100 ℃) of the prepared polyisobutene succinic acid alcohol ester polymer emulsifier finished product for the emulsion explosive is as follows: 215mm2/s, acid value 38mgKOH/g, density (20 ℃ C.): 1225kg/m3, moisture content: 0.06%, minimum critical amount emulsification test: 0.55 percent of the emulsion explosive is prepared according to the formula of the static emulsion and static sensitization emulsion explosive, observed by a polarizing microscope, and obviously crystallized after being stored for 4 months. The produced product is tested on a static emulsification and high-temperature static sensitization production line, and the production process, the sensitization process, the water-oil phase proportion and the like are not changed. And after the test is carried out on the production line, random sampling is carried out to detect the initial performance and the natural storage performance is detected, and the natural storage performance reaches 4 months. The results are as follows:
Figure BDA0002264686510000061
example 3
As shown in fig. 1, a synthesis method of polyisobutylene succinic acid alcohol ester polymer emulsifier for emulsion explosive comprises the following steps:
1) under the protection of nitrogen, 1000kg of high-activity polyisobutylene (with the number average molecular weight of 600) and 225kg of maleic anhydride are subjected to alkylation reaction at 170 ℃ by a thermal heating method for 6 hours to generate a crude product of the polyisobutylene succinic anhydride, a proper amount of n-hexane is added to dissolve the product after the reaction is finished, and the pure polyisobutylene succinic anhydride is obtained by the processes of filtering, vacuumizing, leaching and the like;
2) carrying out esterification reaction on purified polyisobutene succinic anhydride and a certain amount of solvent toluene and glycerol under the action of a high-efficiency catalyst sulfuryl chloride (the adding amount of the catalyst is 0.05-0.15 percent of the total mass) at 90 ℃, wherein the reaction time is 5 hours, and polyisobutene succinic alcohol ester is generated, namely a polyisobutene succinic acid alcohol ester high-molecular emulsifier primary finished product for emulsion explosives;
3) adding a quantitative saturated salt solution into the polyisobutylene succinic acid alcohol ester high molecular emulsifier primary product for the emulsion explosive, removing unreacted glycerol, evaporating the obtained solution, and performing filtration separation and HLB value adjustment to obtain a finished polyisobutylene succinic acid alcohol ester high molecular emulsifier for the emulsion explosive.
In the step 2), the adopted catalyst is sulfuryl chloride, and the adding amount of the catalyst is 0.05-0.1% of the total mass. The mass of the polyisobutylene succinic anhydride (PIBSA) is 200-500% of that of the glycerol.
The product kinematic viscosity (100 ℃) of the prepared polyisobutene succinic acid alcohol ester polymer emulsifier finished product for the emulsion explosive is as follows: 350mm2/s, acid value 33mgKOH/g, density (20 ℃ C.): 1033kg/m3, moisture content: 0.10%, minimum critical amount emulsification test: 0.65 percent, the emulsion explosive is prepared according to the formula of the static emulsion and static sensitization emulsion explosive, observed by a polarizing microscope, and obviously crystallized after being stored for 5 months. The produced product is tested on a static emulsification and high-temperature static sensitization production line, and the production process, the sensitization process, the water-oil phase proportion and the like are not changed. And after the test is carried out on the production line, random sampling is carried out to detect the initial performance and the natural storage performance is detected, and the natural storage performance reaches 5 months. The results are as follows:
Figure BDA0002264686510000071
Figure BDA0002264686510000081
example 4
As shown in fig. 1, a synthesis method of polyisobutylene succinic acid alcohol ester polymer emulsifier for emulsion explosive comprises the following steps:
1) under the protection of nitrogen, 1000kg of high-activity polyisobutylene (with the number average molecular weight of 600) and 225kg of maleic anhydride are subjected to alkylation reaction at 180 ℃ by a thermal heating method for 6.5 hours to generate a crude product of the polyisobutylene succinic anhydride, a proper amount of normal hexane is added to dissolve the product after the reaction is finished, and processes such as filtering, vacuumizing, leaching and the like are carried out to obtain pure polyisobutylene succinic anhydride (PIBSA);
2) carrying out esterification reaction on purified polyisobutylene succinic anhydride (PIBSA) and a certain amount of solvents toluene and glycerol under the action of a high-efficiency catalyst sulfuryl chloride (the adding amount of the catalyst is 0.05-0.15 percent of the total mass) at 135 ℃ for 2.5 hours to generate polyisobutylene succinic alcohol ester, namely a polyisobutylene succinic alcohol ester high-molecular emulsifier primary finished product for the emulsion explosive;
3) adding a quantitative saturated salt solution into the polyisobutylene succinic acid alcohol ester high molecular emulsifier primary product for the emulsion explosive, removing unreacted glycerol, evaporating the obtained solution, and performing filtration separation and HLB value adjustment to obtain a finished polyisobutylene succinic acid alcohol ester high molecular emulsifier for the emulsion explosive.
In the step 2), the adopted catalyst is sulfuryl chloride, and the adding amount of the catalyst is 0.05-0.1% of the total mass. The mass of the polyisobutylene succinic anhydride (PIBSA) is 200-500% of that of the glycerol.
The product kinematic viscosity (100 ℃) of the prepared polyisobutene succinic acid alcohol ester polymer emulsifier finished product for the emulsion explosive is as follows: 330mm2(s), acid value: 31mgKOH/g, density (20 ℃ C.): 1008kg/m3The water content: 0.08%, minimum critical amount emulsification test: 0.6 percent, the emulsion explosive is prepared according to the formula of the static emulsion and static sensitization emulsion explosive, observed by a polarizing microscope, and obviously crystallized after being stored for 5 months. The produced product is tested on a static emulsification and high-temperature static sensitization production line, and the production process, the sensitization process, the water-oil phase proportion and the like are not changed. And after the test is carried out on the production line, random sampling is carried out to detect the initial performance and the natural storage performance is detected, and the natural storage performance reaches 5 months. The results are as follows:
Figure BDA0002264686510000091
example 5
As shown in fig. 1, a synthesis method of polyisobutylene succinic acid alcohol ester polymer emulsifier for emulsion explosive comprises the following steps:
1) under the protection of nitrogen, 1000kg of high-activity polyisobutylene (with the number average molecular weight of 600) and 225kg of maleic anhydride are subjected to alkylation reaction at 180 ℃ by a thermal heating method for 6.5 hours to generate a crude product of the polyisobutylene succinic anhydride, a proper amount of normal hexane is added to dissolve the product after the reaction is finished, and processes such as filtering, vacuumizing, leaching and the like are carried out to obtain pure polyisobutylene succinic anhydride (PIBSA);
2) carrying out esterification reaction on purified polyisobutylene succinic anhydride (PIBSA) and a certain amount of solvents toluene and glycerol under the action of a high-efficiency catalyst sulfuryl chloride (the adding amount of the catalyst is 0.05-0.15% of the total mass) at 135100-150 ℃, wherein the reaction time is 6 hours, and polyisobutylene succinic acid alcohol ester is generated, namely a polyisobutylene succinic acid alcohol ester high-molecular emulsifier primary finished product for emulsion explosives;
3) adding a quantitative saturated salt solution into the polyisobutylene succinic acid alcohol ester high molecular emulsifier primary product for the emulsion explosive, removing unreacted glycerol, evaporating the obtained solution, and performing filtration separation and HLB value adjustment to obtain a finished polyisobutylene succinic acid alcohol ester high molecular emulsifier for the emulsion explosive.
In the step 2), the adopted catalyst is sulfuryl chloride, and the adding amount of the catalyst is 0.05-0.1% of the total mass. The mass of the polyisobutylene succinic anhydride (PIBSA) is 200-500% of that of the glycerol.
The product kinematic viscosity (100 ℃) of the prepared polyisobutene succinic acid alcohol ester polymer emulsifier finished product for the emulsion explosive is as follows: 268mm2/s, acid value 25mgKOH/g, density (20 ℃ C.): 960kg/m3, moisture content: 0.02%, minimum critical amount emulsification test: 0.25 percent, the emulsion explosive is prepared according to the formula of the static emulsion and static sensitization emulsion explosive, observed by a polarizing microscope, and obviously crystallized after being stored for 12 months. The produced product is tested on a static emulsification and high-temperature static sensitization production line, and the production process, the sensitization process, the water-oil phase proportion and the like are not changed. After the test is carried out on the production line, the random sampling is carried out to detect the initial performance and the natural storage performance is detected, and the natural storage performance can reach 12 months. The results are as follows:
Figure BDA0002264686510000101
Figure BDA0002264686510000111

Claims (8)

1. a synthetic method of a polyisobutylene succinic acid alcohol ester high molecular emulsifier for emulsion explosives is characterized by comprising the following steps:
1) the first step is that polyisobutylene and maleic anhydride are subjected to thermal addition reaction to prepare polyisobutylene succinic anhydride;
carrying out alkylation reaction on polyisobutylene and maleic anhydride at 160-220 ℃ for 4-7 hours by a thermal heating method to generate a crude polyisobutylene succinic anhydride product, adding a proper amount of normal hexane to dissolve the product after the reaction is finished, and carrying out filtration, vacuumizing, leaching and other processes to obtain pure polyisobutylene succinic anhydride;
2) and (2) carrying out esterification reaction on the purified polyisobutylene succinic anhydride, toluene and glycerol serving as solvents under the action of sulfuryl chloride at the temperature of 100-150 ℃, wherein the reaction time is 3-8 hours, and polyisobutylene succinic acid alcohol ester is generated and is a polyisobutylene succinic acid alcohol ester high-molecular emulsifier primary product for the emulsion explosive.
2. The method for synthesizing the polyisobutylene succinic acid ester high molecular emulsifier for the emulsion explosive according to claim 1, wherein the method for synthesizing the polyisobutylene succinic acid ester high molecular emulsifier further comprises the following steps:
adding saturated salt water into the primary product of the polyisobutylene succinic acid alcohol ester high molecular emulsifier for the emulsion explosive, removing unreacted glycerol, evaporating the obtained solution, and performing filtering separation and HLB value adjustment to obtain the finished product of the polyisobutylene succinic acid alcohol ester high molecular emulsifier for the emulsion explosive.
3. The method for synthesizing the polyisobutylene succinic acid ester high molecular emulsifier for the emulsion explosive according to claim 1 or 2, which is characterized in that: in the step 1), the polyisobutene is high-activity polyisobutene.
4. The method for synthesizing the polyisobutylene succinic acid ester high molecular emulsifier for the emulsion explosive according to claim 1 or 2, which is characterized in that: in the step 1), polyisobutylene and maleic anhydride are subjected to a heating method under the protection of nitrogen to produce high-content polyisobutylene succinic anhydride.
5. The method for synthesizing the polyisobutylene succinic acid ester high molecular emulsifier for the emulsion explosive according to claim 1 or 2, which is characterized in that: in the step 2), the adding amount of sulfuryl chloride is 0.05 to 0.15 percent of the total mass.
6. The method for synthesizing the polyisobutylene succinic acid ester high molecular emulsifier for the emulsion explosive according to claim 1 or 2, which is characterized in that: in the step 2), the mass of the polyisobutylene succinic anhydride is 200-500% of that of the glycerol.
7. The method for synthesizing the polyisobutylene succinic acid ester high molecular emulsifier for the emulsion explosive according to claim 2, which is characterized in that: the mass of the saturated salt water is 0.04-0.06% of the mass of the polyisobutylene succinic acid ester high molecular emulsifier primary product for the emulsion explosive.
8. The method for synthesizing the polyisobutylene succinic acid ester high molecular emulsifier for the emulsion explosive according to claim 2, which is characterized in that: the HLB value is 3-6.
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113024334A (en) * 2021-03-24 2021-06-25 葛洲坝易普力湖北昌泰民爆有限公司 Oil phase for preparing medium-low temperature sensitization process emulsion explosive by using coal-to-liquid intermediate product and preparation method thereof
CN115558044A (en) * 2022-09-30 2023-01-03 北矿亿博(沧州)科技有限责任公司 Crosslinkable polymer emulsifier and preparation method thereof, latex matrix and emulsion explosive

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0994087A2 (en) * 1998-10-16 2000-04-19 Clariant GmbH Explosives containing modified copolymers made from polyisobutylene and maleic anhydride as emulsifier
US20060223945A1 (en) * 2003-01-21 2006-10-05 Hollingshurst Claire L Low color polyisobutylene succinic anhydride-derived emulsifiers
CN105348416A (en) * 2015-11-03 2016-02-24 葛洲坝易普力股份有限公司 Novel emulsion explosive polymer emulsifier and preparation method thereof
CN106008760A (en) * 2016-05-12 2016-10-12 葛洲坝易普力湖北昌泰民爆有限公司 Synthesis method for lipid polymer emulsifier for emulsion explosives
CN106045797A (en) * 2016-05-24 2016-10-26 江南大学 Emulsifying agent for emulsion explosive, and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0994087A2 (en) * 1998-10-16 2000-04-19 Clariant GmbH Explosives containing modified copolymers made from polyisobutylene and maleic anhydride as emulsifier
US20060223945A1 (en) * 2003-01-21 2006-10-05 Hollingshurst Claire L Low color polyisobutylene succinic anhydride-derived emulsifiers
CN105348416A (en) * 2015-11-03 2016-02-24 葛洲坝易普力股份有限公司 Novel emulsion explosive polymer emulsifier and preparation method thereof
CN106008760A (en) * 2016-05-12 2016-10-12 葛洲坝易普力湖北昌泰民爆有限公司 Synthesis method for lipid polymer emulsifier for emulsion explosives
CN106045797A (en) * 2016-05-24 2016-10-26 江南大学 Emulsifying agent for emulsion explosive, and preparation method thereof

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
习锟: "聚异丁烯丁二酸二乙二醇酯的合成及其在乳化炸药中的应用", 《中国优秀博硕士学位论文全文数据库(硕士)工程科技Ⅰ辑》 *
刘永明,等: "高分子酯类乳化剂在乳化炸药中的应用", 《山西化工》 *
黄正华,等: "聚异丁烯丁二酸醇酯高分子乳化剂合成探讨", 《煤矿爆破》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113024334A (en) * 2021-03-24 2021-06-25 葛洲坝易普力湖北昌泰民爆有限公司 Oil phase for preparing medium-low temperature sensitization process emulsion explosive by using coal-to-liquid intermediate product and preparation method thereof
CN113024334B (en) * 2021-03-24 2022-04-22 葛洲坝易普力湖北昌泰民爆有限公司 Oil phase for preparing medium-low temperature sensitization process emulsion explosive by using coal-to-liquid intermediate product and preparation method thereof
CN115558044A (en) * 2022-09-30 2023-01-03 北矿亿博(沧州)科技有限责任公司 Crosslinkable polymer emulsifier and preparation method thereof, latex matrix and emulsion explosive

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