CN114249917A - Ammonium stearate suspension with high saponification rate and production method thereof - Google Patents
Ammonium stearate suspension with high saponification rate and production method thereof Download PDFInfo
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- CN114249917A CN114249917A CN202111446234.5A CN202111446234A CN114249917A CN 114249917 A CN114249917 A CN 114249917A CN 202111446234 A CN202111446234 A CN 202111446234A CN 114249917 A CN114249917 A CN 114249917A
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0014—Use of organic additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
- C08K5/098—Metal salts of carboxylic acids
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Abstract
The invention discloses an ammonium stearate suspension with high saponification rate and a production method thereof. The ammonium stearate suspension with high saponification rate is prepared with stearic acid 20-35 weight portions, emulsifier 1-3 weight portions, ammonia water 10-20 weight portions, alkali catalyst 0.1-0.5 weight portions and water 42-69 weight portions; stearic acid is prepared into oil-in-water stearic acid nano emulsion, and the oil-in-water stearic acid nano emulsion reacts with ammonia water under the action of an alkaline catalyst to finally prepare ammonium stearate suspension with the saponification rate of more than 95%. The ammonium stearate suspension has the characteristics of high saponification rate (the saponification rate is more than 95%), low viscosity (the room-temperature viscosity is lower than 100mPas), good storage stability and stable product performance, has the characteristic of low consumption and high efficiency when being used as a foam stabilizing foaming agent, and has high practical value.
Description
Technical Field
The invention relates to the technical field of chemical additives, in particular to an ammonium stearate suspension with high saponification rate and a production method thereof.
Background
In recent years, waterborne polyurethane and polyacrylic acid foaming systems are widely used for preparing foaming coatings such as synthetic leather and advertising cloth due to environmental protection. Ammonium stearate is often widely used as a foaming foam stabilizer in aqueous polymer foaming coatings due to its superior foam stabilization property, an ammonium stearate suspension is generally prepared by saponification of stearic acid and ammonia water (as disclosed in patent applications CN200710067469.7, CN200910096656.7 and CN 201810733925.5), the above process for preparing ammonium stearate generally performs saponification at 30-40 ℃, although the reaction temperature is low, the following problems are generally encountered, stearic acid is in the form of micron solid particles and incompletely reacts with ammonia water, so that the saponification rate is not high (about 50%), and unreacted stearic acid particles are dispersed in an aqueous phase to form an emulsion, so that the final product has high viscosity, poor fluidity and low emulsion stability. Because the saponification rate is low, the foaming and foam stabilizing efficiency is not high, and more amount of the soap solution needs to be added to play a role in foam stabilization.
Disclosure of Invention
The purpose of the invention is as follows: in order to solve the technical problems, the invention provides an ammonium stearate suspension with high saponification rate and a production method thereof.
The technical scheme is as follows: the technical scheme of the invention is to provide an ammonium stearate suspension with high saponification rate, which is prepared from the following raw materials, by weight, 20-35 parts of stearic acid, 1-3 parts of an emulsifier, 10-20 parts of ammonia water, 0.1-0.5 part of an alkaline catalyst and 42-69 parts of water; stearic acid is prepared into oil-in-water stearic acid nano emulsion, and the oil-in-water stearic acid nano emulsion reacts with ammonia water under the action of an alkaline catalyst to finally prepare ammonium stearate suspension with the saponification rate of more than 95 percent, wherein the viscosity of the ammonium stearate suspension is lower than 100mPas at room temperature.
Preferably, the stearic acid is industrial grade and contains saturated fatty acid of C16-C18.
Preferably, the emulsifier is at least one of an anionic surfactant and a nonionic surfactant.
Further preferably, the anionic surfactant is at least one of fatty alcohol sulfate, alkyl sulfonate, fatty acid salt and fatty alcohol ether phosphate; the nonionic surfactant is at least one of fatty alcohol-polyoxyethylene ether, alkylphenol polyoxyethylene ether, sorbitan fatty acid ester polyoxyethylene ether and fatty acid monoglyceride.
Further preferably, the anionic surfactant is at least one of sodium dodecyl sulfate, sodium dodecyl sulfate and potassium lauryl alcohol ether phosphate; the nonionic surfactant is at least one of glyceryl monostearate, sorbitan stearate and sorbitan oleate polyoxyethylene ether.
Preferably, the concentration of the ammonia water is 25 to 28%.
Preferably, the alkaline catalyst is at least one of sodium hydroxide and potassium hydroxide, and is prepared into a 20% solution when in use.
Preferably, the water is deionized water.
The preparation method of the ammonium stearate suspension with high saponification rate comprises the following steps:
(1) mixing stearic acid and an oil-soluble emulsifier, and heating to 60-75 ℃ to obtain an oil phase liquid; mixing water with water-soluble emulsifier, and heating to 60-75 deg.C to obtain water phase liquid;
(2) adding the water phase liquid into the oil phase liquid, controlling the temperature at 60-75 ℃, the stirring speed at 300-500rpm, and the emulsifying time at 3-10min to obtain stearic acid primary emulsion, and then obtaining nano stearic acid emulsion through high-pressure micro-jet treatment;
(3) and (3) adding an aqueous solution of an alkaline catalyst into the nano stearic acid emulsion obtained in the step (2), and dropwise adding ammonia water for 10-30min, controlling the temperature to be 35-45 ℃, and reacting for 1-3h to obtain the ammonium stearate suspension with the high saponification rate.
Preferably, the temperature in the step (1) and the temperature in the step (2) are both controlled at 70 ℃, and the emulsifying time in the step (2) is 5 min.
The invention principle is as follows: according to the invention, stearic acid is prepared into the oil-in-water type nano emulsion, and then reacts with ammonia water under the action of the alkaline catalyst, so that the contact area between the alkali liquor and stearic acid is greatly increased, the saponification rate is greatly improved, the viscosity of the ammonium stearate suspension is reduced, and the stability of the system is increased.
Has the advantages that: compared with the prior art, the invention has the following remarkable advantages: (1) the preparation process of the ammonium stearate suspension can obviously improve the saponification rate of stearic acid; (2) the ammonium stearate suspension of the invention has low viscosity and high stability; (3) when the ammonium stearate suspension is used as a foam stabilizing foaming agent, the ammonium stearate suspension has the characteristic of low dosage and high efficiency.
Detailed Description
The technical solution of the present invention is further illustrated by the following examples.
Example 1
The ammonium stearate suspension comprises the following raw materials in percentage by mass: 25 parts of stearic acid, 1 part of sodium dodecyl sulfate, 1 part of sorbitan monostearate, 12 parts of 25% ammonia water, 0.3 part of potassium hydroxide and 61 parts of water.
The preparation method of the ammonium stearate suspension specifically comprises the following steps:
(1) weighing 25 parts of stearic acid and 1 part of sorbitan monostearate in a stirring kettle, stirring and heating to 70 ℃ to obtain an oil phase liquid.
(2) Weighing 1 part of sodium dodecyl sulfate and 59.8 parts of water, placing the sodium dodecyl sulfate and the water in another container, heating to 70 ℃, and stirring to obtain an aqueous phase liquid.
(3) Adding the liquid obtained in the step (2) into the stirring kettle obtained in the step (1) while the liquid is hot, mixing and stirring at the rotating speed of 400rpm for 5min to obtain stearic acid primary emulsion, and then carrying out high-pressure micro-jet treatment to obtain nano stearic acid emulsion;
(4) and (4) adding 0.3 part of 20% aqueous solution prepared from potassium hydroxide into the nano stearic acid emulsion obtained in the step (3), dropwise adding 12 parts of 25% ammonia water for 10min, controlling the temperature to be 35 ℃, and reacting for 1.5h to obtain the ammonium stearate suspension with the high saponification rate.
Example 2
The ammonium stearate suspension comprises the following raw materials in percentage by mass: 30 parts of stearic acid, 1.5 parts of sodium dodecyl sulfate, 1 part of stearic acid monoglyceride, 15 parts of 25% ammonia water, 0.5 part of sodium hydroxide and 53 parts of water.
The preparation method of the ammonium stearate suspension specifically comprises the following steps:
(1) weighing 30 parts of stearic acid and 1 part of stearic acid monoglyceride into a stirring kettle, stirring and heating to 70 ℃ to obtain an oil phase liquid.
(2) Weighing 1.5 parts of sodium dodecyl sulfate and 51 parts of water, placing the mixture in another container, heating to 70 ℃, and stirring to obtain an aqueous phase liquid.
(3) Adding the liquid obtained in the step (2) into the stirring kettle obtained in the step (1) while the liquid is hot, mixing and stirring at the rotating speed of 300rpm for 5min to obtain stearic acid primary emulsion, and then carrying out high-pressure micro-jet treatment to obtain nano stearic acid emulsion;
(4) and (4) adding 0.5 part of 20% aqueous solution prepared from sodium hydroxide into the nano stearic acid emulsion obtained in the step (3), dropwise adding 15 parts of 25% ammonia water for 15min, controlling the temperature at 40 ℃, and reacting for 2h to obtain the ammonium stearate suspension with the high saponification rate.
Example 3
The ammonium stearate suspension comprises the following raw materials in percentage by mass: 35 parts of stearic acid, 2 parts of sorbitan monooleate polyoxyethylene ether, 1 part of stearic acid monoglyceride, 20 parts of 25% ammonia water, 0.5 part of potassium hydroxide and 42 parts of water.
The preparation method of the ammonium stearate suspension specifically comprises the following steps:
(1) weighing 35 parts of stearic acid and 1 part of stearic acid monoglyceride into a stirring kettle, and heating to 70 ℃ to obtain an oil phase liquid.
(2) Weighing 2 parts of sorbitan monooleate polyoxyethylene ether and 40 parts of water, placing the weighed materials in another container, heating to 70 ℃, and stirring to obtain an aqueous phase liquid.
(3) Adding the liquid obtained in the step (2) into the stirring kettle obtained in the step (1) while the liquid is hot, mixing and stirring at the rotating speed of 500rpm for 5min to obtain stearic acid primary emulsion, and then carrying out high-pressure micro-jet treatment to obtain nano stearic acid emulsion;
(4) and (4) adding 0.5 part of 20% aqueous solution prepared from potassium hydroxide into the nano stearic acid emulsion obtained in the step (3), dropwise adding 20 parts of 25% ammonia water for 30min, controlling the temperature to be 35 ℃, and reacting for 3h to obtain the high saponification rate ammonium stearate suspension.
Example 4
The ammonium stearate suspension comprises the following raw materials in percentage by mass: 20 parts of stearic acid, 1 part of potassium lauryl alcohol ether phosphate, 10 parts of 28% ammonia water, 0.1 part of potassium hydroxide and 69 parts of water.
The preparation method of the ammonium stearate suspension specifically comprises the following steps:
(1) weighing 20 parts of stearic acid in a stirring kettle, and heating to 70 ℃ to obtain an oil phase liquid.
(2) 1 part of potassium lauryl alcohol ether phosphate and 68.6 parts of water are weighed and placed in another container, the temperature is raised to 70 ℃, and stirring is carried out, so as to obtain aqueous phase liquid.
(3) Adding the liquid obtained in the step (2) into the stirring kettle obtained in the step (1) while the liquid is hot, mixing and stirring at the rotating speed of 300rpm for 5min to obtain stearic acid primary emulsion, and then carrying out high-pressure micro-jet treatment to obtain nano stearic acid emulsion;
(4) and (4) adding 0.1 part of 20% aqueous solution prepared from potassium hydroxide into the nano stearic acid emulsion obtained in the step (3), and dropwise adding 10 parts of 28% ammonia water for 10min, controlling the temperature at 45 ℃ and reacting for 2h to obtain the high saponification rate ammonium stearate suspension.
Comparative example (prior art):
the ammonium stearate emulsion comprises the following raw materials in parts by mass: 25 parts of stearic acid, 3 parts of sodium dodecyl sulfate, 12 parts of 25% ammonia water and 60 parts of water.
Sequentially adding stearic acid, sodium dodecyl sulfate and water into a reaction container, adjusting the temperature to 40 ℃, starting a stirrer, stirring uniformly, slowly adding ammonia water, stirring at a high speed of 1400 rpm until stearic acid is completely dispersed, reacting for 3h, transferring the liquid into an emulsification tank, emulsifying at a high speed of 3000 rpm for 30min, standing for 1-2 h, and filtering to obtain the ammonium stearate emulsion.
The products prepared in examples 1-4 and comparative example were tested and the results are shown in Table 1.
TABLE 1
| Analysis item | Example 1 | Example 2 | Example 3 | Example 4 | Comparative example |
| Saponification ratio (%) | 96.5 | 97 | 96 | 99 | 45 |
| Viscosity (25 ℃, mPas) | 90 | 95 | 100 | 85 | 620 |
| Stability (30 days) | Not layering | Not layering | Not layering | Not layering | With a layer separation |
From the above test results, it can be seen that the present invention has the following significant advantages compared to the prior art (comparative example): the preparation process of the ammonium stearate suspension can obviously improve the saponification rate of stearic acid by more than 100 percent compared with the saponification rate of the prior art, and the ammonium stearate suspension prepared by the invention has the characteristics of low viscosity and high stability, and has high use level, low efficiency and high practical value when being used as a foam stabilizing foaming agent.
Claims (10)
1. The ammonium stearate suspension with high saponification rate is characterized by being prepared from the following raw materials in parts by weight: 20-35 parts of stearic acid, 1-3 parts of emulsifier, 10-20 parts of ammonia water, 0.1-0.5 part of alkaline catalyst and 42-69 parts of water; stearic acid is prepared into oil-in-water stearic acid nano emulsion, and the oil-in-water stearic acid nano emulsion reacts with ammonia water under the action of an alkaline catalyst to finally prepare ammonium stearate suspension with the saponification rate of more than 95%.
2. The ammonium stearate suspension with high saponification rate of claim 1, wherein the stearic acid is technical grade and contains saturated fatty acid C16-C18.
3. The ammonium stearate suspension with high saponification rate according to claim 1, wherein the emulsifier is at least one of an anionic surfactant and a nonionic surfactant.
4. The ammonium stearate suspension with high saponification rate of claim 3, wherein the anionic surfactant is at least one of fatty alcohol sulfate, alkyl sulfonate, fatty acid salt, fatty alcohol ether phosphate salt; the nonionic surfactant is at least one of fatty alcohol-polyoxyethylene ether, alkylphenol polyoxyethylene ether, sorbitan fatty acid ester polyoxyethylene ether and fatty acid monoglyceride.
5. The ammonium stearate suspension with high saponification rate of claim 4, wherein the anionic surfactant is at least one of sodium dodecyl sulfate, and potassium lauryl ether phosphate; the nonionic surfactant is at least one of glyceryl monostearate, sorbitan stearate and sorbitan oleate polyoxyethylene ether.
6. The ammonium stearate suspension having a high saponification rate of claim 1, wherein the ammonia concentration is 25-28%.
7. The ammonium stearate suspension with high saponification rate of claim 1, wherein the alkaline catalyst is at least one of sodium hydroxide and potassium hydroxide.
8. The ammonium stearate suspension with a high saponification rate of claim 1, wherein the ammonium stearate suspension has a viscosity of less than 100mPas at room temperature.
9. The method for preparing an ammonium stearate suspension with a high saponification rate according to any one of claims 1 to 8, comprising the steps of:
(1) mixing stearic acid and an oil-soluble emulsifier, and heating to 60-75 ℃ to obtain an oil phase liquid; mixing water with water-soluble emulsifier, and heating to 60-75 deg.C to obtain water phase liquid;
(2) adding the water phase liquid into the oil phase liquid, controlling the temperature at 60-75 ℃, the stirring speed at 300-500rpm, and the emulsifying time at 3-10min to obtain stearic acid primary emulsion, and then obtaining nano stearic acid emulsion through high-pressure micro-jet treatment;
(3) and (3) adding an alkaline catalyst into the nano stearic acid emulsion obtained in the step (2), and dropwise adding ammonia water for 10-30min, controlling the temperature to be 35-45 ℃, and reacting for 1-3h to obtain the ammonium stearate suspension with the high saponification rate.
10. The method for preparing an ammonium stearate suspension with a high saponification rate as claimed in claim 9, wherein the temperature in step (1) and step (2) is controlled at 70 ℃ and the emulsification time in step (2) is 5 min.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4664844A (en) * | 1984-01-19 | 1987-05-12 | Basf Aktiengesellschaft | Antifoams based on oil-in-water emulsions |
| CN101508857A (en) * | 2009-03-12 | 2009-08-19 | 宋金火 | Ammonium stearate emulsion and producing method thereof |
| CN104961372A (en) * | 2015-06-10 | 2015-10-07 | 广东首诚建设科技有限公司 | Setting time-adjustable waterproof foam stabilizer and preparation method thereof |
| CN110305521A (en) * | 2019-05-28 | 2019-10-08 | 桐乡市宏源化工厂(普通合伙) | A kind of foam stabiliser and preparation method thereof having no irritating odor |
| CN112647306A (en) * | 2020-11-10 | 2021-04-13 | 扬州大学 | Solid-liquid mixed type foam stabilizer and preparation method thereof |
-
2021
- 2021-11-30 CN CN202111446234.5A patent/CN114249917B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4664844A (en) * | 1984-01-19 | 1987-05-12 | Basf Aktiengesellschaft | Antifoams based on oil-in-water emulsions |
| CN101508857A (en) * | 2009-03-12 | 2009-08-19 | 宋金火 | Ammonium stearate emulsion and producing method thereof |
| CN104961372A (en) * | 2015-06-10 | 2015-10-07 | 广东首诚建设科技有限公司 | Setting time-adjustable waterproof foam stabilizer and preparation method thereof |
| CN110305521A (en) * | 2019-05-28 | 2019-10-08 | 桐乡市宏源化工厂(普通合伙) | A kind of foam stabiliser and preparation method thereof having no irritating odor |
| CN112647306A (en) * | 2020-11-10 | 2021-04-13 | 扬州大学 | Solid-liquid mixed type foam stabilizer and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 黄政宇等: "硬脂酸铵乳液和表面活性剂复配体系的泡沫性能研究与应用", 《化工进展》 * |
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