CN113441079A - Method for synthesizing dimer acid emulsifier - Google Patents
Method for synthesizing dimer acid emulsifier Download PDFInfo
- Publication number
- CN113441079A CN113441079A CN202010217821.6A CN202010217821A CN113441079A CN 113441079 A CN113441079 A CN 113441079A CN 202010217821 A CN202010217821 A CN 202010217821A CN 113441079 A CN113441079 A CN 113441079A
- Authority
- CN
- China
- Prior art keywords
- dimer acid
- steps
- reaction
- emulsifier
- following
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B23/00—Compositions characterised by non-explosive or non-thermic constituents
- C06B23/009—Wetting agents, hydrophobing agents, dehydrating agents, antistatic additives, viscosity improvers, antiagglomerating agents, grinding agents and other additives for working up
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)
Abstract
The invention discloses a method for synthesizing a dimer acid emulsifier, which comprises the following steps: (1) adding dimer acid into a reactor, stirring and heating to 80 ℃, and starting a vacuum pump; (2) adding polyalcohol and catalyst solution, continuously heating to 190 ℃ at 150 ℃, stirring for reaction for 2-5 hours, and controlling the heating speed at 20-30 ℃/h to obtain an intermediate containing aliphatic groups; (3) cooling the intermediate containing the aliphatic group in the step (2) to 120 ℃, adding a diluent, then adding polyamine or alcohol amine, controlling the temperature to be 120-180 ℃ for reaction, stirring and reacting for 1-2 hours in a vacuum state, controlling the temperature rise speed to be 10-20 ℃/h, and stopping the reaction after all water generated by the reaction is evaporated; (4) cooling and discharging to obtain the emulsifier with the content of more than 70%. The emulsifier is used for industrial colloidal explosives, the emulsibility of the product in the preparation process is greatly improved, the emulsion can be smoothly emulsified in a state of reducing the stirring strength in the emulsion preparation process, the emulsifier has a certain self-emulsifying function, and the stability of the colloid is greatly improved after the emulsion is finished.
Description
Technical Field
The invention relates to a preparation method of an emulsifier, in particular to a synthesis method of a dimer acid emulsifier.
Background
Dimer acid is a dibasic acid produced by addition polymerization of two molecules of C8 unsaturated fatty acid, such as oleic acid, linoleic acid, etc., contains two polar carboxyl groups and a larger nonpolar hydrocarbon group, has chemical properties similar to fatty acid, contains two carboxyl groups in the molecule, can perform various reactions such as lipidation, amination, etc., has larger alkyl groups and 1-3 double bonds in the molecule, and can perform chemical reactions such as addition, polymerization, etc. Dimer acids are generally used in the fields of resins, cosmetics, lubricants and the like. The emulsifier currently used for industrial colloidal explosives is S-80 or polyisobutylene succinimide high molecular emulsifier (the former has poor stability, and the latter has poor emulsibility), but because an oil phase and a water phase exist simultaneously in the production of the industrial colloidal explosives, the density difference is large, the acidity of a nitrate supersaturated solution is low, and on the other hand, because of the performance requirement of oxygen balance in the industrial explosives, the addition amount of the emulsifier and oil phase materials is low, so that the industrial colloidal explosives have the defects of poor emulsibility, high safety risk during emulsification, harsh emulsification conditions, poor product stability and the like in the preparation process at present and need to be improved. The invention provides a method for synthesizing a dimer acid emulsifier, and the prepared dimer acid emulsifier can solve the defects and completely meet the performance requirements of industrial colloidal explosives.
Disclosure of Invention
The invention provides a method for synthesizing a dimer acid emulsifier to solve the defects.
The above object of the present invention is achieved by the following technical means: a method for synthesizing dimer acid emulsifier comprises the following steps:
(1) adding dimer acid into a reactor, stirring and heating to 80 ℃, starting a vacuum pump, and keeping the vacuum degree at 50-700 mmHg;
(2) adding polyol and a catalyst solution, continuously heating to 190 ℃ at 150 ℃, stirring for reaction for 2-5 hours, and controlling the heating speed at 20-30 ℃/h to obtain an intermediate containing aliphatic groups, namely dimer acid polyol ester;
(3) cooling the intermediate containing the aliphatic group in the step (2), namely dimer acid polyol ester, to 120 ℃, adding a diluent, then adding polyamine or alcohol amine, controlling the temperature to be 120-180 ℃ for reaction, stirring and reacting for 1-2 hours in a vacuum state, controlling the temperature rise speed to be 10-20 ℃/h, and stopping the reaction after all water generated by the reaction is evaporated;
(4) cooling and discharging to obtain the emulsifier with the content of more than 70%.
Further, the reactor is provided with a mechanical stirrer, a condenser, a vacuum device and a thermometer.
Further, the mass ratio of the dimer acid to the polyol is 100: 10-30.
Further, the mass ratio of the dimer acid polyol ester to the polyamine or the alcohol amine is 100: 5-40.
Furthermore, the adding amount of the catalyst is 0.1-1 per mill; the catalyst is NaOH or KOH aqueous solution, and the concentration of the catalyst solution is 30%.
Further, the addition amount of the diluent is 50% of the dimer acid, and the diluent is vegetable oil.
Further, the polyhydric alcohol is any one or more of ethylene glycol, polyethylene glycol, butanediol, hexanediol, glycerol, pentaerythritol, butanetriol, cyclohexanol, sorbitol, inositol and mannitol.
Furthermore, the polyamine and the alcohol amine are any one or more of polymethylene polyamine, polyethylene polyamine, polypropylene polyamine, diethylenetriamine, ethylenediamine, triethylene tetramine, tetraethylenepentamine, monoethanolamine, diethanolamine, monoethanol diisopropanolamine, triisopropanolamine, triaminomethane and glucosamine.
The emulsifier is suitable for W/O type emulsion, has special effect on industrial colloidal explosive, and has the characteristics of safety, environmental protection and stable colloid storage.
Compared with the prior art, the invention has the advantages that:
(1) the emulsifier is prepared by carrying out esterification and amination reaction on the dimer acid, is used for industrial colloidal explosives, greatly improves the emulsibility in the preparation process of the product, can be smoothly emulsified in a state of reducing the stirring strength in the emulsion preparation process, has a certain self-emulsifying function, and greatly improves the stability of the colloid after the emulsification is finished.
(2) The preparation process of the emulsifier has no by-product and precipitate, complete reaction and stable product quality.
(3) The diluent used in the preparation process does not need to be separated and can be used for emulsifying the external phase material of the product, thereby reducing the cost of the product.
(4) The product can be mixed with vegetable oil, paraffin and resin, and can be stored in liquid state for a long time without precipitation and separation, and can be prepared into solutions with different concentrations according to user requirements, and is suitable for products with different use requirements.
(5) The product has no special requirement on equipment during industrial production.
Detailed Description
The present invention will be described in more detail with reference to examples.
Example 1: a method for synthesizing dimer acid emulsifier comprises adding 500g of high-purity dimer acid into a reactor with a mechanical stirrer, a condenser, a vacuum device and a thermometer, stirring and heating to 80 ℃, adding 100g of diethylene glycol and 0.5g of NaOH solution, starting a stirring and vacuum pump, keeping the vacuum degree at 50-100mmHg, slowly heating, keeping the vacuum state and the stirring state at 130 ℃, controlling the heating rate at 10-20 ℃/h to gradually evaporate formed water, keeping the temperature for reaction for 1h when the temperature is 190 ℃, closing the vacuum pump, slowly cooling to 150 ℃, adding diluent oil, cooling to 90 ℃, adding tetraethylenepentamine, starting the stirring and vacuum pump, slowly heating at 8-10 ℃/h, keeping the reaction for 1h when the temperature is 130 ℃, sampling and measuring the acid value to be less than 1mg/g, and obtaining a light yellow transparent emulsifier after the reaction is finished.
Example 2: a method for synthesizing dimer acid emulsifier comprises adding 500g of high-purity dimer acid into a reactor with a mechanical stirrer, a condenser, a vacuum device and a thermometer, stirring and heating to 80 ℃, adding 110g of glycerol and 0.6g of NaOH solution, starting a stirring and vacuum pump, keeping the vacuum degree at 100-, and obtaining a light yellow transparent emulsifier after the reaction is finished.
Example 3: a method for synthesizing dimer acid emulsifier comprises adding 500g of high-purity dimer acid into a reactor with a mechanical stirrer, a condenser, a vacuum device and a thermometer, stirring and heating to 80 ℃, adding 130g of sorbitol and 1g of NaOH solution, starting a stirring and vacuum pump, keeping the vacuum degree at 50-200mmHg, slowly heating, keeping the vacuum state and the stirring state at the temperature of 130 ℃, controlling the heating speed at 10-20 ℃/h to gradually evaporate formed water, keeping the temperature for reaction for 2h when the temperature is increased to 190 ℃, closing the vacuum pump, slowly cooling to 120 ℃, adding diluent oil, cooling to 90 ℃, adding ethylenediamine, starting the stirring and vacuum pump, slowly heating at the temperature rising speed of 8-10 ℃/h, keeping the reaction for 1h when the temperature is increased to 140 ℃, sampling and determining the acid value to be less than 1mg/g, and obtaining a light yellow transparent emulsifier after the reaction is finished.
The emulsifier can adapt to W/O type emulsion of various materials in various proportions, can be widely applied to the industrial fields of cosmetics, textiles and the like, and particularly shows excellent performance when applied to industrial colloidal explosives.
The industrial gel explosive has the following characteristics, and the selection of the emulsifying agent is limited:
A. the industrial colloidal explosive is a W/O type emulsion, wherein the water phase is a nitrate supersaturated solution, the concentration of the solution is as high as 95 percent, generally between 80 and 95 percent, the crystallization point of the solution is between 60 and 100 ℃, the solution is in a solid state at normal temperature, the pH value is between 4 and 5, and the density is between 1.35 and 1.45g/cm during thin-film fertilization. The oil phase is composed of lubricating oil, vaseline, paraffin, microcrystalline wax and an emulsifier, the density of the oil phase is generally between 0.8 and 0.9 g/cm, the oil phase is liquid or solid at normal temperature, the density and acidity difference between the water phase and the oil phase is large, and the water phase and the oil phase need to be heated to be above the melting point for emulsification.
B. The industrial colloidal explosive is limited by danger and safety in the preparation process, so that the lower the stirring strength is required to be, the better the stirring strength is, the larger the emulsifier gap is, and the conditions of temperature rise, friction and direct impact are not required in the emulsification process.
C. The performance requirement of the industrial colloidal explosive is that the oxygen balance value is based on zero oxygen, and positive oxygen or negative oxygen deviating from the zero oxygen balance can influence the performance and can generate toxic and harmful gases with different degrees during blasting, so that the ratio of the water phase to the oil phase is controlled to be 90-96: 9-4, and the use amount of the emulsifier and the oil phase is limited to be not too high.
It can be understood that the oil phase with the density of about 5 percent and 0.8g/cm is subjected to an emulsification process to emulsify the nitrate aqueous solution with the density of about 95 percent and 1.4g/cm into an emulsion composed of water-in-oil type small particles with the emulsion particle size of 1-2 microns, and the stability of the emulsion is required to be not less than half a year.
The emulsifier used by the industrial colloidal explosive at present is S-80 or polyisobutylene succinimide high molecular emulsifier, the former has poor stability, and the latter has insufficient emulsibility.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes performed by the present invention in the specification and the content of the embodiment, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (8)
1. A method for synthesizing dimer acid emulsifier is characterized by comprising the following steps: the method comprises the following steps:
(1) adding dimer acid into a reactor, stirring and heating to 80 ℃, starting a vacuum pump, and keeping the vacuum degree at 50-700 mmHg;
(2) adding polyol and a catalyst solution, continuously heating to 190 ℃ at 150 ℃, stirring for reaction for 2-5 hours, and controlling the heating speed at 20-30 ℃/h to obtain an intermediate containing aliphatic groups, namely dimer acid polyol ester;
(3) cooling the intermediate containing the aliphatic group in the step (2), namely dimer acid polyol ester, to 120 ℃, adding a diluent, then adding polyamine or alcohol amine, controlling the temperature to be 120-180 ℃ for reaction, stirring and reacting for 1-2 hours in a vacuum state, controlling the temperature rise speed to be 10-20 ℃/h, and stopping the reaction after all water generated by the reaction is evaporated;
(4) cooling and discharging to obtain the emulsifier with the content of more than 70%.
2. The method for synthesizing dimer acid emulsifier according to claim 1, wherein the method comprises the following steps: the reactor is provided with a mechanical stirrer, a condenser, a vacuum device and a thermometer.
3. The method for synthesizing dimer acid emulsifier according to claim 1, wherein the method comprises the following steps: the mass ratio of the dimer acid to the polyhydric alcohol is 100: 10-30.
4. The method for synthesizing dimer acid emulsifier according to claim 1, wherein the method comprises the following steps: the mass ratio of the dimer acid polyol ester to the polyamine or the alcohol amine is 100: 5-40.
5. The method for synthesizing dimer acid emulsifier according to claim 1, wherein the method comprises the following steps: the addition amount of the catalyst is 0.1-1 per mill; the catalyst is NaOH or KOH aqueous solution, and the concentration of the catalyst solution is 30%.
6. The method for synthesizing dimer acid emulsifier according to claim 1, wherein the method comprises the following steps: the addition amount of the diluent is 50 percent of the dimer acid, and the diluent is vegetable oil.
7. The method for synthesizing dimer acid emulsifier according to claim 1, wherein the method comprises the following steps: the polyalcohol is one or more of ethylene glycol, polyethylene glycol, butanediol, hexanediol, glycerol, pentaerythritol, butanetriol, cyclohexanol, sorbitol, inositol, and mannitol.
8. The method for synthesizing dimer acid emulsifier according to claim 1, wherein the method comprises the following steps: the polyamine and the alcohol amine are any one or more of polymethylene polyamine, polyethylene polyamine, polypropylene polyamine, diethylenetriamine, ethylenediamine, triethylene tetramine, tetraethylenepentamine, monoethanolamine, diethanolamine, monoethanol diisopropanolamine, triisopropanolamine, triaminomethane and glucosamine.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010217821.6A CN113441079A (en) | 2020-03-25 | 2020-03-25 | Method for synthesizing dimer acid emulsifier |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010217821.6A CN113441079A (en) | 2020-03-25 | 2020-03-25 | Method for synthesizing dimer acid emulsifier |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113441079A true CN113441079A (en) | 2021-09-28 |
Family
ID=77806873
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010217821.6A Pending CN113441079A (en) | 2020-03-25 | 2020-03-25 | Method for synthesizing dimer acid emulsifier |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113441079A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114426815A (en) * | 2022-01-18 | 2022-05-03 | 中国石油化工股份有限公司 | Oil-based drilling fluid suitable for strong water-sensitive and easily-collapsed stratum and preparation method and application thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4420349A (en) * | 1982-02-02 | 1983-12-13 | C-I-L Inc. | Emulsion explosive compositions and method of preparation |
| US4836870A (en) * | 1987-10-01 | 1989-06-06 | Mitchell Chemical Co. | Emulsion-type explosive compositions |
| CN101983222A (en) * | 2008-02-04 | 2011-03-02 | 比克化学股份有限公司 | Wetting and dispersing agent |
| CN102976877A (en) * | 2012-12-24 | 2013-03-20 | 江南大学 | Novel emulsifier for emulsion explosive and preparation method of novel emulsifier |
| CN106163492A (en) * | 2014-04-11 | 2016-11-23 | 巴斯夫欧洲公司 | The mixture of cosmetic UV absorbers |
| CN110028998A (en) * | 2018-01-12 | 2019-07-19 | 雅富顿化学公司 | For the emulsifier in lubricating oil |
-
2020
- 2020-03-25 CN CN202010217821.6A patent/CN113441079A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4420349A (en) * | 1982-02-02 | 1983-12-13 | C-I-L Inc. | Emulsion explosive compositions and method of preparation |
| US4836870A (en) * | 1987-10-01 | 1989-06-06 | Mitchell Chemical Co. | Emulsion-type explosive compositions |
| CN101983222A (en) * | 2008-02-04 | 2011-03-02 | 比克化学股份有限公司 | Wetting and dispersing agent |
| CN102976877A (en) * | 2012-12-24 | 2013-03-20 | 江南大学 | Novel emulsifier for emulsion explosive and preparation method of novel emulsifier |
| CN106163492A (en) * | 2014-04-11 | 2016-11-23 | 巴斯夫欧洲公司 | The mixture of cosmetic UV absorbers |
| CN110028998A (en) * | 2018-01-12 | 2019-07-19 | 雅富顿化学公司 | For the emulsifier in lubricating oil |
Non-Patent Citations (1)
| Title |
|---|
| 卞克建: "《工业化学反应及应用》", 28 February 1999 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114426815A (en) * | 2022-01-18 | 2022-05-03 | 中国石油化工股份有限公司 | Oil-based drilling fluid suitable for strong water-sensitive and easily-collapsed stratum and preparation method and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| EP1017925B1 (en) | Method and compound for inhibiting the plugging of conduits by gas hydrates | |
| US4395266A (en) | Stabilized water-in-mineral oil emulsion | |
| CA1217891A (en) | Stabilization of tackifying resin dispersions | |
| JPS63203645A (en) | Process for producing basic salts, salts produced and oil compositions containing salts of this kind | |
| FR2692283A1 (en) | Acid-anhydride esters as oil field corrosion inhibitors (Ester anhidride acid as corrosion inhibitor in the field of oils). | |
| FR3070162B1 (en) | POLYESTERAMINES AND POLYESTERQUATS | |
| WO1989004856A1 (en) | Water reducible soft coating compositions | |
| CN113441079A (en) | Method for synthesizing dimer acid emulsifier | |
| CN115161643B (en) | Nanometer silicon corrosion inhibitor containing benzotriazole and preparation method thereof | |
| US8481622B2 (en) | Soybean based epoxy resin and methods of making and use | |
| JPH05507114A (en) | Stable polyamide resin microdispersions, methods for their preparation and transparent continuous films formed from microdispersions | |
| CN113443947A (en) | Dimer acid emulsifier | |
| CN104355994B (en) | A kind of aryl alkyl polyols ester and application thereof | |
| KR102138579B1 (en) | Manufacturing method of self-emulsifiying hydrogenated vegetable oil using glycerine fatty acid and cosmetic composition including the same | |
| CN109554203A (en) | A kind of preparation method of emulsion resistance Low sulfur diesel antiwear additive | |
| JP5864381B2 (en) | Novel fluorocarbon chain-containing compound, its production method and use | |
| US2987491A (en) | Alkyd resins modified by beta amino crotonic esters of higher organic hydroxides | |
| CN113750578B (en) | Amide polymer molecular-level defoaming agent and preparation method thereof | |
| CN102718613B (en) | Half-esterification high polymer emulsifying agent for industrial explosives | |
| CN110862471A (en) | Method for synthesizing polyisobutylene succinic acid alcohol ester high-molecular emulsifier for emulsion explosive | |
| CN108699491B (en) | Amide of aliphatic polyamine and 12-hydroxyoctadecanoic acid and lipase-stabilized thickener composition | |
| EP1802565B1 (en) | Process for preparing hydroxy functional vegetable oils | |
| KR20230038208A (en) | resin dispersion composition | |
| Pham et al. | Synthesis of surfactants by polymerization of glycerol (meth) acrylates with fatty acids derivatives as chain ends | |
| EP0759916A1 (en) | Explosive compositions |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210928 |