CN113493532B - Emulsifier for remote delivery of latex matrix and preparation method and application thereof - Google Patents
Emulsifier for remote delivery of latex matrix and preparation method and application thereof Download PDFInfo
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- CN113493532B CN113493532B CN202110891999.3A CN202110891999A CN113493532B CN 113493532 B CN113493532 B CN 113493532B CN 202110891999 A CN202110891999 A CN 202110891999A CN 113493532 B CN113493532 B CN 113493532B
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- C—CHEMISTRY; METALLURGY
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Abstract
The invention discloses an emulsifier for latex matrix remote distribution and a preparation method and application thereof, wherein the emulsifier comprises polyolefin carboxylic anhydride, alcohol or polyoxyethylene alkyl ether, dihydrazide and diluent oil, and the molar ratio of the polyolefin carboxylic anhydride, the alcohol or polyoxyethylene alkyl ether and the dihydrazide is 1.0:0.5 to 1.2:0.5 to 1.2, wherein the mass of the diluent oil is 0.3 to 1 time of that of the polyolefin carboxylic anhydride; the preparation method comprises the following steps: s1, adding polyolefin carboxylic anhydride into a reaction kettle; s2, introducing protective gas into the reaction kettle; s3, adding alcohol or polyoxyethylene alkyl ether into the reaction kettle, adding diluent oil, heating to 100-120 ℃, and preserving heat for 2-3 hours; s4, adding dihydrazide under protective gas, heating to 160-180 ℃, and stirring for 4-6 h under heat preservation; s5, filtering while the mixture is hot, wherein the obtained filtrate is a finished product of the emulsifier; the latex matrix prepared by the emulsifier has good fluidity, stable storage, excellent anti-bumping performance and pumping resistance, and is suitable for the remote delivery of the latex matrix.
Description
Technical Field
The invention relates to the technical field of industrial explosive production, in particular to an emulsifier for latex matrix remote distribution and a preparation method and application thereof.
Background
The emulsifier is used as a key component in the emulsion explosive, and the type, performance index and content of the emulsifier have obvious influence on the quality, the size, the stability and the detonation performance of an emulsion system.
The low molecular emulsifier represented by Span-80 has high emulsifying efficiency and low costIs cheap and can meet the production of the conventional emulsion explosive, but emulsion particles form micelles, and the interface forms a film which is not tightly packed, because the formed film is very thin (the thickness is about the thickness)
) And an elastic frame structure is not provided, so that the interfacial film has insufficient elasticity, is easy to age and crack, has poor stability and short product storage period.
The emulsion particles in the emulsion system formed by the macromolecular emulsifier represented by the polyisobutylene succinic anhydride derivative form micelles, the interface forms a macromolecular framework and a well-accumulated monomolecular interfacial film, and the emulsion system has good elasticity, strong elasticity and large thickness (reaching the thickness of the macromolecular emulsifier)
). Because the particles form a three-dimensional barrier film and are charged with the same kind of charges, electrostatic repulsion is generated among the particles, the anti-agglomeration structure is favorable for improving the stability, and the product has a long storage period.
Patents US20060223945A1 and CN1158833A disclose polyisobutylene succinate emulsifier using glycerin as esterification reagent, CN1186078, US4225589, US6770605, US4119553 and the like disclose polyisobutylene succinate emulsifier using pentaerythritol as esterification reagent, and US3381022 discloses polyisobutylene succinate emulsifier using ethylene glycol as esterification reagent.
The latex matrix prepared by the high-molecular emulsifying agent has good storage stability, but has poor bumping resistance and pumping resistance, high dynamic viscosity at normal temperature, large yield stress, poor fluidity and difficult pumping, and the long-distance distribution of the latex matrix is difficult to realize due to the defects.
Disclosure of Invention
The invention aims to provide an emulsifier for remote delivery of latex matrix, and a preparation method and application thereof.
In order to achieve the above purpose, the invention provides the following technical scheme:
an emulsifier for remote dispensing of latex matrix, which comprises polyolefin carboxylic anhydride, alcohol or polyoxyethylene alkyl ether, dihydrazide and diluent oil, wherein the molar ratio of the polyolefin carboxylic anhydride, the alcohol or polyoxyethylene alkyl ether and the dihydrazide is 1.0:0.5 to 1.2:0.5 to 1.2, and the mass of the diluent oil is 0.3 to 1 time of that of the polyolefin carboxylic anhydride.
According to the technical scheme, alcohol or polyoxyethylene alkyl ether is adopted for directional ring opening and mono-esterification, then the di-hydrazide reaction is carried out on the di-esterified fatty alcohol or polyoxyethylene alkyl ether, enough hydrophilic groups are introduced, and the hydrophilic-lipophilic balance is achieved between the di-esterified fatty alcohol and the hydrophilic groups, so that the obtained emulsifier has good emulsifying property and emulsifying stability, and the prepared latex matrix has good storage stability, anti-bumping and pumping-resistant properties.
Further, the polyolefin carboxylic acid anhydride is any one of polyethylene succinic anhydride, polypropylene succinic anhydride, polybutylene succinic anhydride, polyisobutylene succinic anhydride and polypentene succinic anhydride; the molecular weight of the polyolefin chain in the polyolefin carboxylic anhydride is 500-2000.
Further, the alcohol is C3-C10 polyalcohol or polyglycerol, and the polymerization degree n of the polyglycerol is 3-6.
Further, the polyoxyethylene alkyl ether has an oxyethylene group number of 3 to 8 and an alkyl group number of 11 to 15.
Further, the structural formula of the dihydrazide is shown in the specification
Wherein R is a carbon chain of C5-C12.
Through the technical scheme, due to the existence of C5-C12 carbon chains in the dihydrazide structure, the rigidity of the molecular structure is obviously reduced, the dynamic viscosity and the yield stress of the prepared latex matrix are obviously reduced, the excellent fluidity and the pumping performance are shown, and the method is very suitable for the development of centralized preparation and remote distribution modes of the latex matrix.
A method of preparing an emulsifier for remote delivery of a latex matrix, comprising the steps of: s1, adding polyolefin carboxylic anhydride into a reaction kettle; s2, introducing protective gas into the reaction kettle; s3, adding alcohol or polyoxyethylene alkyl ether into the reaction kettle, adding diluent oil, heating to 100-120 ℃, and preserving heat for 2-3 hours; s4, adding dihydrazide under protective gas, heating to 160-180 ℃, and stirring for 4-6 h under heat preservation; s5, filtering while the mixture is hot, wherein the obtained filtrate is the finished product of the emulsifier.
By adopting the technical scheme, the carbonization can be effectively prevented by adding the protective gas, and the generation of impurities is reduced; the heating temperature is 100-120 ℃, and the heat preservation is carried out for 2-3h, so that only the mono-esterification but not the multi-esterification can be controlled; after the dihydrazide is added, the reaction is kept at the temperature of 160-180 ℃ and stirred for 4-6 h, so that the yield of the dihydrazide product is over 90 percent.
Further, the protective gas is an inert gas.
The emulsifier for remote delivery of the emulsion matrix prepared by the preparation method is applied to explosives.
Compared with the prior art, the invention has the beneficial effects that:
an emulsifier for latex matrix remote distribution, which comprises polyolefin carboxylic anhydride, alcohol or polyoxyethylene alkyl ether, dihydrazide and diluent oil, wherein the mole ratio of the polyolefin carboxylic anhydride, the alcohol or polyoxyethylene alkyl ether and the dihydrazide is 1.0:0.5 to 1.2:0.5 to 1.2, and the mass of the diluent oil is 0.3 to 1.2 times of that of the polyolefin carboxylic anhydride; alcohol or polyoxyethylene alkyl ether is adopted for directional ring opening and mono-esterification, then the di-hydrazide reaction is carried out on the mono-esterification and the di-hydrazide reaction, enough hydrophilic groups are introduced, and the hydrophilic-lipophilic balance is achieved with the lipophilic groups, so that the obtained emulsifier has good emulsifying property and emulsifying stability, and the prepared latex matrix has good storage stability and bumping and pumping resistance;
the structural formula of the dihydrazide is
Wherein R is a C5-C12 carbon chain; due to the existence of C5-C12 carbon chains in the dihydrazide structure, the rigidity of the molecular structure is obviously reduced, the dynamic viscosity and the yield stress of the prepared latex matrix are obviously reduced, the prepared latex matrix has excellent fluidity and pumping performance, and the method is very suitable for being used for preparing the emulsion matrixThe development of centralized preparation and remote distribution modes of the latex matrix.
Detailed Description
The present invention will be described in further detail with reference to test examples and specific embodiments. It should be understood that the scope of the above-described subject matter of the present invention is not limited to the following examples, and any technique realized based on the contents of the present invention is within the scope of the present invention.
The raw material sources are all commercially available.
Further, the polyolefin carboxylic acid anhydride is any one of polyethylene succinic anhydride, polypropylene succinic anhydride, polybutylene succinic anhydride, polyisobutylene succinic anhydride and polypentene succinic anhydride; the polyolefin chain in the polyolefin carboxylic anhydride has a molecular weight of 500-2000.
Further, the alcohol is a C3-C10 polyol or polyglycerol, and the degree of polymerization n of the polyglycerol is 3-6.
Further, the polyoxyethylene alkyl ether has an oxyethylene group number of 3 to 8 and an alkyl group having 11 to 15 carbon atoms.
Further, the structural formula of the dihydrazide is shown in the specification
Wherein R is a carbon chain of C5-C12.
Examples
Example 1
The emulsifier of the embodiment is prepared from the following raw materials: the polyolefin carboxylic acid anhydride is polypropylene succinic anhydride, the alcohol is neopentyl glycol, the dihydrazide is adipic hydrazide, and the diluent oil is 60SN base oil.
A method of preparing an emulsifier for remote delivery of a latex matrix, comprising the steps of:
s1, adding 1mol of polypropylene succinic anhydride into a reaction kettle;
s2, introducing ammonia gas into the reaction kettle;
s3, adding 1.1mol of neopentyl glycol into a reaction kettle, weighing the 60SN base oil to enable the mass of the 60SN base oil to be 0.8 time that of 1mol of polypropylene succinic anhydride, then adding the 60SN base oil, heating to 120 ℃, and preserving heat for 2 hours;
s4, heating to 170 ℃, adding 0.8mol of adipic dihydrazide under ammonia gas, and stirring for 4 hours under heat preservation;
and S5, filtering while the mixture is hot to obtain a finished product.
Example 2
The emulsifier of the embodiment comprises the following raw materials: the polyolefin carboxylic acid anhydride is polyisobutylene succinic anhydride, the alcohol is 1, 6-hexanediol, the dihydrazide is glutaryl hydrazine, and the diluent oil is 220SN base oil.
A method of preparing an emulsifier for remote delivery of a latex matrix, comprising the steps of:
s1, adding 1mol of polyisobutylene succinic anhydride into a reaction kettle;
s2, introducing ammonia gas into the reaction kettle;
s3, adding 1.2mol of 1, 6-hexanediol into a reaction kettle, weighing the weight of 220SN base oil to ensure that the mass of the 220SN base oil is the same as that of 1mol of polyisobutylene succinic anhydride, then adding the 220SN base oil, heating to 110 ℃, and preserving heat for 3 hours;
s4, heating to 160 ℃, adding 0.7mol of glutaryl hydrazine under ammonia gas, and stirring for 6 hours under heat preservation;
and S5, filtering while the mixture is hot to obtain a finished product.
Example 3
The emulsifier of the embodiment is prepared from the following raw materials: the polyolefin carboxylic acid anhydride is selected from the group consisting of poly (pentylene succinic anhydride), the alcohol is selected from the group consisting of trimethylolpropane, the dihydrazide is selected from the group consisting of pimeloyl dihydrazide, and the diluent oil is selected from the group consisting of 150SN base oil.
A method of preparing an emulsifier for remote delivery of a latex matrix, comprising the steps of:
s1, adding 1mol of poly (glutaric anhydride) into a reaction kettle;
s2, introducing ammonia gas into the reaction kettle;
s3, adding 1mol of trimethylolpropane into a reaction kettle, weighing 150SN base oil to enable the weight of the 150SN base oil to be 0.5 time that of 1mol of polyglutamic acid anhydride, then adding the 150SN base oil, heating to 120 ℃, and preserving heat for 3 hours;
s4, heating to 180 ℃, adding 1mol of pimeloyl dihydrazide under ammonia gas, and stirring for 4 hours under heat preservation;
and S5, filtering while the mixture is hot to obtain a finished product.
Example 4
The emulsifier of the embodiment comprises the following raw materials: the polyolefin carboxylic acid anhydride is polybutylene succinic anhydride, the polyoxyethylene alkyl ether is polyoxyethylene pentadecyl (4) ether, the dihydrazide is adipyl, and the diluent oil is 150SN base oil.
A method of preparing an emulsifier for remote delivery of a latex matrix, comprising the steps of:
s1, adding 1mol of polybutylene succinic anhydride into a reaction kettle;
s2, introducing ammonia gas into the reaction kettle;
s3, adding 0.8mol of polyoxyethylene pentadecyl (4) ether into a reaction kettle, weighing 150SN base oil to enable the weight of the 150SN base oil to be 0.5 time that of 1mol of the polyglutamic acid anhydride, then adding 150SN base oil, heating to 120 ℃, and preserving heat for 2 hours;
s4, heating to 170 ℃, adding 1mol of adipic dihydrazide under ammonia gas, and stirring for 4 hours under the condition of heat preservation;
and S5, filtering while the mixture is hot to obtain a finished product.
Example 5
The emulsifier of the embodiment comprises the following raw materials: the polyolefin carboxylic acid anhydride is polyisobutylene succinic anhydride, the polyoxyethylene alkyl ether is polyoxyethylene dodecyl (7) ether, the dihydrazide is glutaryl hydrazide, and the diluent oil is 60SN base oil.
A method of preparing an emulsifier for remote delivery of a latex matrix, comprising the steps of:
s1, adding 1mol of polyisobutylene succinic anhydride into a reaction kettle;
s2, introducing ammonia gas into the reaction kettle;
s3, adding 1mol of polyoxyethylene dodecyl (7) ether into a reaction kettle, wherein the weight of 60SN base oil is 0.7 times of that of 1mol of polyisobutylene succinic anhydride, adding 60SN base oil, heating to 110 ℃, and preserving heat for 3 hours;
s4, heating to 160 ℃, adding 0.7mol of glutaryl hydrazine in ammonia gas, and stirring for 6 hours under the condition of heat preservation;
and S5, filtering while the mixture is hot to obtain a finished product.
Example 6
The emulsifier of the embodiment comprises the following raw materials: the polyolefin carboxylic acid anhydride is polypentaolefin succinic anhydride, the polyoxyethylene alkyl ether is polyoxyethylene tridecyl (5) ether, the dihydrazide is pimelic hydrazide, and the diluent oil is 150SN base oil.
A method of preparing an emulsifier for remote delivery of a latex matrix, comprising the steps of:
s1, adding 1mol of poly (glutaric anhydride) into a reaction kettle;
s2, introducing ammonia gas into the reaction kettle;
s3, adding 1.2mol of polyoxyethylene tridecyl (5) ether into a reaction kettle, weighing 150SN base oil to ensure that the mass of the 150SN base oil is the same as that of 1mol of the polyglutame olefin succinic anhydride, then adding the 150SN base oil, heating to 120 ℃, and preserving heat for 3 hours;
s4, heating to 180 ℃, adding 1mol of pimeloyl dihydrazide under ammonia gas, and stirring for 4 hours under heat preservation;
and S5, filtering while the mixture is hot to obtain a finished product.
Example 7
The emulsifier of the embodiment is prepared from the following raw materials: the polyolefin carboxylic acid anhydride is polypropylene succinic anhydride, the alcohol is triglycerol, the dihydrazide is adipamide, and the diluent oil is 60SN base oil.
A method of preparing an emulsifier for remote delivery of a latex matrix, comprising the steps of:
s1, adding 1mol of polypropylene succinic anhydride into a reaction kettle;
s2, introducing ammonia gas into the reaction kettle;
s3, adding 0.5mol of triglycerin into the reaction kettle, weighing the 60SN base oil to enable the mass of the 60SN base oil to be 0.8 times that of 1mol of polypropylene succinic anhydride, then adding the 60SN base oil, heating to 100 ℃, and preserving heat for 2.5 hours;
s4, heating to 160 ℃, adding 0.8mol of adipic dihydrazide under ammonia gas, and stirring for 4 hours under heat preservation;
and S5, filtering while the mixture is hot to obtain a finished product.
Example 8
The emulsifier of the embodiment is prepared from the following raw materials: the polyolefin carboxylic acid anhydride is polyisobutylene succinic anhydride, the alcohol is tetrapolyglycerol, the dihydrazide is glutaryl hydrazide, and the diluent oil is 150SN base oil.
A method of preparing an emulsifier for remote delivery of a latex matrix, comprising the steps of:
s1, adding 1mol of polyisobutylene succinic anhydride into a reaction kettle;
s2, introducing ammonia gas into the reaction kettle;
s3, adding 0.7mol of tetraglycerol into a reaction kettle, weighing the 220SN base oil to enable the mass of 150SN base oil to be 0.5 time of that of 1mol of polyisobutylene succinic anhydride, then adding 150SN base oil, heating to 110 ℃, and preserving heat for 3 hours;
s4, heating to 170 ℃, adding 1mol of glutaryl hydrazine in ammonia gas, and stirring for 6 hours under the condition of heat preservation;
and S5, filtering while the mixture is hot to obtain a finished product.
Example 9
The emulsifier of the embodiment is prepared from the following raw materials: the polyolefin carboxylic acid anhydride is selected from the group consisting of polypentaolefin succinic anhydride, alcohol is selected from the group consisting of hexaglycerol, dihydrazide is selected from the group consisting of pimeloyl dihydrazide, and the diluent oil is selected from the group consisting of 220SN base oil.
A method of preparing an emulsifier for remote delivery of a latex matrix, comprising the steps of:
s1, adding 1mol of poly (glutaric anhydride) into a reaction kettle;
s2, introducing ammonia gas into the reaction kettle;
s3, adding 1mol of hexaglycerol into a reaction kettle, weighing the weight of 220SN base oil to enable the mass of the 220SN base oil to be 0.3 times that of 1mol of poly (pentylene succinic anhydride), then adding the 220SN base oil, heating to 120 ℃, and preserving heat for 3 hours;
s4, heating to 180 ℃, adding 1.2mol of pimeloyl dihydrazide under ammonia gas, and stirring for 6 hours under heat preservation;
and S5, filtering while the mixture is hot to obtain a finished product.
Comparative example
A commercially available T154 emulsifier is selected.
Application example
The emulsion matrices prepared from the emulsifiers of examples 1 to 9 and comparative example were tested to prepare formed explosives.
Performance test
The performance of the emulsion matrix and the performance of the mixed emulsion explosive are tested, and the test results are shown in the following table 1:
TABLE 1 emulsion matrix Performance and Mixed emulsion explosive Performance Table prepared by emulsifier
Compared with the comparative examples, the emulsifying agent disclosed by the invention has good emulsifying property and emulsifying stability, the prepared emulsion matrix has low normal-temperature dynamic viscosity, small yield stress, good fluidity, easiness in pumping, stability in storage, excellent bumping resistance and pumping resistance, the field charging and blasting after remote distribution, the blasting speed in a hole is more than 5800m/s, the overall performance is excellent, and the emulsifying agent is very suitable for the centralized preparation and remote distribution modes of the emulsion matrix.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (7)
1. An emulsifier for remote delivery of a latex matrix, comprising: the emulsifier comprises polyolefin carboxylic anhydride, polyoxyethylene alkyl ether, dihydrazide and diluent oil, wherein the mole ratio of the polyolefin carboxylic anhydride, the polyoxyethylene alkyl ether and the dihydrazide is 1.0:0.5 to 1.2:0.5 to 1.2, wherein the mass of the diluent oil is 0.3 to 1 time of that of the polyolefin carboxylic anhydride; the polyolefin carboxylic acid anhydride is any one of polyethylene succinic anhydride, polypropylene succinic anhydride, polybutylene succinic anhydride, polyisobutylene succinic anhydride and polypentene succinic anhydride.
2. The emulsion of claim 1, wherein: the molecular weight of the polyolefin chain in the polyolefin carboxylic anhydride is 500-2000.
3. The emulsion of claim 1, wherein: the polyoxyethylene alkyl ether has an oxyethylene group number of 3 to 8 and an alkyl group number of 11 to 15.
4. An emulsifier for remote delivery of a latex matrix as claimed in claim 1, wherein: the structural formula of the dihydrazide is
Wherein R is a carbon chain of C5-C12.
5. A method of preparing an emulsifier for remote delivery of a latex matrix according to any of claims 1 to 4, comprising the steps of: s1, adding polyolefin carboxylic anhydride into a reaction kettle; s2, introducing protective gas into the reaction kettle; s3, adding polyoxyethylene alkyl ether into the reaction kettle, adding diluent oil, heating to 100-120 ℃, and preserving heat for 2-3 hours; s4, adding dihydrazide under protective gas, heating to 160-180 ℃, and stirring for 4-6 h under heat preservation; s5, filtering while the mixture is hot, wherein the obtained filtrate is the finished product of the emulsifier.
6. The method of claim 5, wherein the emulsifier is selected from the group consisting of: the protective gas is inert gas.
7. Use of an emulsifier for remote delivery of an emulsion matrix, wherein the emulsifier produced by the method of claim 5 or 6 is used in an explosive.
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| US7160944B2 (en) * | 2003-06-17 | 2007-01-09 | Crompton Corporation | Process for the preparation of a polyolefin emulsion and hybrid polyolefin-polyurethane dispersion derived therefrom |
| DE102006013898A1 (en) * | 2006-03-25 | 2007-09-27 | Celanese Emulsions Gmbh | Polymer dispersions containing two copolymers with different glass transition points and a non-ionic emulsifier of the aryl-substituted alkoxylated phenol ether type, used in paint or varnish for wood and other substrates |
| CN105384946B (en) * | 2015-11-03 | 2018-03-20 | 葛洲坝易普力股份有限公司 | Low sheraing emulsification macromolecule emulsifier and preparation method thereof |
| CN105968236A (en) * | 2016-06-14 | 2016-09-28 | 中国葛洲坝集团易普力股份有限公司 | Novel emulgator for emulsified explosive and preparation method of novel emulgator |
| CN106084096A (en) * | 2016-06-14 | 2016-11-09 | 中国葛洲坝集团易普力股份有限公司 | emulsifier for emulsion explosive and preparation method thereof |
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| Title |
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| Influences of octamethylenedicarboxylic dibenzoylhydrazide on crystallization, melting behaviors, and properties of isotactic polypropylene;Zhang, YF等;《POLYMER BULLETIN》;20190430;第76卷(第4期);第1685-1696页 * |
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