CN114438816A - Oil-in-water type high-carbon alcohol emulsion composition and preparation method thereof - Google Patents
Oil-in-water type high-carbon alcohol emulsion composition and preparation method thereof Download PDFInfo
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- CN114438816A CN114438816A CN202210109873.0A CN202210109873A CN114438816A CN 114438816 A CN114438816 A CN 114438816A CN 202210109873 A CN202210109873 A CN 202210109873A CN 114438816 A CN114438816 A CN 114438816A
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
- D21H21/06—Paper forming aids
- D21H21/12—Defoamers
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/03—Non-macromolecular organic compounds
- D21H17/05—Non-macromolecular organic compounds containing elements other than carbon and hydrogen only
- D21H17/14—Carboxylic acids; Derivatives thereof
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Abstract
The application discloses an oil-in-water high-carbon alcohol emulsion composition and a preparation method thereof. The composition comprises the following components in percentage by weight: 10-25% of fatty alcohol with high carbon number, 1-5% of fatty alcohol with low carbon number, 1-3% of fatty acid, 0.05-0.2% of catalyst, 0.5-5% of nonionic surfactant, 0.5-5% of thickening agent and the balance of water; wherein the fatty alcohol with high carbon number is C18-C30 fatty alcohol, and the acid value range is 0.05-1.0mg KOH/g; the fatty alcohol with low carbon number is C12-C16 fatty alcohol; the fatty acid is C12-C22 fatty acid. The invention introduces fatty acid and fatty alcohol with low carbon number, the fatty alcohol with low carbon number and the introduced fatty acid are subjected to esterification reaction, the fatty acid remained in the fatty alcohol with low carbon number and the fatty alcohol with high carbon number are subjected to esterification reaction, and the introduced fatty acid and the fatty alcohol with high carbon number are subjected to esterification reaction, so that the generated mixed esterified substance has the effect of emulsifying and stabilizing the fatty alcohol with high carbon number, and simultaneously improves the degassing performance of the product in different use temperature environments.
Description
Technical Field
The invention belongs to the technical field of degasifying agents used in papermaking processes, and particularly relates to an oil-in-water high-carbon alcohol emulsion composition and a preparation method thereof.
Background
Oil-in-water type higher alcohol emulsion compositions have been widely used as deaerators in papermaking processes. This type of degassing agent generally has two drawbacks, namely, on the one hand, the viscosity of the product increases during storage and even solidifies, which can cause inconvenience to the consumer during use of the product, and on the other hand, the degassing properties of the product are greatly affected by the temperature of the environment in which it is used, and severely show completely different performance effects in winter and summer.
CN106075961A discloses an emulsion defoaming agent consisting of fatty alcohol, organic hydrocarbon, water-soluble 2-acrylamide-2-methylpropanesulfonic acid homopolymer and/or salt, water-soluble alcohol and non-cationic surfactant, wherein the product stabilizes fatty alcohol emulsion and inhibits viscosity increase through introducing the water-soluble homopolymer, but the product does not solve the problem that the degassing performance of the product is influenced by the temperature of the use environment.
US7763664B2 discloses an oil-in-water dispersion of at least one bisamide of an alcohol of at least 12 carbon atoms, a polyglycerol ester, ethylenediamine and a carboxylic acid of 10 to 36 carbon atoms as the hydrophobic phase, which product has improved degassing properties at high temperatures, but at the same time has an impact on the properties of the product at low temperatures and the product exhibits a tendency to thicken during storage.
JP2000300908A discloses an emulsion of a C12-C30 fatty alcohol, a wax, a fine hydrophobic powder, a thickener and an emulsifier, which improves the instantaneous defoaming properties of the product, but which undergoes thickening during storage.
US5807502A discloses a dispersion of a C10-C28 fatty alcohol, an anionic surfactant, a C6-C18 fatty glycol polyoxyethylene ether and water, which improves the stability of the product during storage by the C6-C18 fatty glycol polyoxyethylene ether, but which does not solve the problem that the degassing properties of the product are affected by the temperature of the use environment.
Therefore, the existing product can not simultaneously and effectively solve the problems that the viscosity of the product is increased during storage and the product performance is influenced by the temperature of the use environment, and can not completely meet the use requirement.
Disclosure of Invention
Aiming at the defects in the prior art, the technical problem to be solved by the application is to provide an oil-in-water type high alcohol emulsion composition which can effectively solve the problems that the viscosity of the product is increased during storage and the product performance is influenced by the use temperature environment. Another technical problem to be solved by the present application is to provide a method for preparing the above oil-in-water type higher alcohol emulsion composition.
In order to solve the technical problem, the technical scheme adopted by the application is as follows:
an oil-in-water type high alcohol emulsion composition comprises the following components in percentage by weight: 10-25% of fatty alcohol with high carbon number, 1-5% of fatty alcohol with low carbon number, 1-3% of fatty acid, 0.05-0.2% of catalyst, 0.5-5% of nonionic surfactant, 0.5-5% of thickening agent and the balance of water; wherein the fatty alcohol with high carbon number is C18-C30 fatty alcohol, and the acid value range is 0.05-1.0mg KOH/g; the fatty alcohol with low carbon number is C12-C16 fatty alcohol; the fatty acid is C12-C22 fatty acid.
The high carbon number fatty alcohol is C18-C30 fatty alcohol, such as single C18 alcohol, single C20 alcohol, single C22 alcohol, single C24 alcohol, single C26 alcohol, single C28 alcohol, single C30 alcohol, C18-C26 mixed alcohol, C24-C28 mixed alcohol, and C20-C28 mixed alcohol, and one or more of them can be selected. Wherein the acid value of the fatty alcohol with high carbon number is 0.05-1.0mg KOH/g.
The low-carbon fatty alcohol is C12-C16 fatty alcohol, such as single C12 alcohol, single C14 alcohol, single C16 alcohol, C12-C16 mixed alcohol, and C12-C14 mixed alcohol, and one or more of them can be selected.
The fatty acid is C12-C22 fatty acid, and can be saturated fatty acid or unsaturated fatty acid, such as monolauric acid, myristic acid, palmitic acid, stearic acid, arachidic acid, behenic acid, and oleic acid, and one or more of them can be selected.
The catalyst is selected from one of concentrated sulfuric acid, concentrated hydrochloric acid and p-toluenesulfonic acid. The catalyst is mainly used for promoting the reaction among fatty acid and fatty acid remained in fatty alcohol with low carbon number, fatty alcohol with high carbon number and fatty alcohol with high carbon number.
The emulsifier is nonionic surfactant, and can be polyoxyethylene alkylphenol, polyoxyethylene fatty alcohol, polyoxyethylene fatty acid, such as polyoxyethylene (20) nonylphenol ether, polyoxyethylene (20) stearyl ether, polyoxyethylene (20) stearate, polyoxyethylene (20) oleate, polyoxyethylene (20) castor oil ether, polyoxyethylene sorbitan monostearate, sorbitan monooleate, sorbitan tristearate, sorbitan trioleate, ethylene glycol stearate, ethylene glycol laurate, propylene glycol oleate, propylene glycol stearate, glycerol monostearate, glycerol monolaurate, diethylene glycol monolaurate, pentaerythritol stearate, polyoxyethylene (20) sorbitan monooleate, polyoxyethylene (20) sorbitan tristearate, polyethylene glycol 4000 monooleate, polyoxyethylene (20) sorbitan tristearate, polyoxyethylene (4000) monooleate, polyoxyethylene (20) sorbitan monooleate, polyoxyethylene (20) polyoxyethylene sorbitan tristearate, polyoxyethylene glycol 4000 monooleate, polyoxyethylene glycol, polyoxyethylene sorbitan monooleate, polyoxyethylene (20) polyoxyethylene sorbitan monooleate, polyoxyethylene (20) polyoxyethylene, Polyethylene glycol 2000 monolaurate, and one or more of them can be selected.
The thickening agent comprises hydroxyethyl cellulose, carboxymethyl cellulose, xanthan gum, polyacrylamide and polyacrylic acid.
The balance of the emulsion composition is water, wherein the water accounts for 60-85% of the total amount of the emulsion.
The preparation method of the oil-in-water type high alcohol emulsion comprises the following steps:
1) mixing and stirring high-carbon fatty alcohol, low-carbon fatty alcohol, fatty acid and a catalyst under the protection of nitrogen, heating to 150 ℃ and 180 ℃, and preserving heat for 3 hours;
2) cooling the mixture obtained in the step 1) to 90-100 ℃, adding an emulsifier, preserving heat and stirring for 30 min;
3) slowly adding water with the temperature of 70-100 ℃ into the mixture obtained in the step 2), preserving the temperature and stirring for 30 min;
4) and 3) passing the mixture obtained in the step 3) through high-speed shearing equipment, cooling to room temperature, and adding a thickening agent to obtain the target product.
Has the advantages that: compared with the prior art, the application has the advantages that:
1) in the components of the oil-in-water type high-carbon alcohol emulsion composition, high-carbon fatty alcohol is a main degassing substance, low-carbon fatty alcohol and introduced fatty acid react with residual fatty acid in the high-carbon fatty alcohol to form an esterified substance, the esterified substance can be used as an emulsifier to stabilize the high-carbon fatty alcohol, and the esterified substance has better degassing performance at different use temperatures.
2) In the application, the fatty acid is used for reacting with the fatty alcohol with low carbon number and the fatty alcohol with high carbon number, and compared with the method for directly introducing the fatty alcohol fatty ester, the method disclosed by the invention has better storage stability and degassing performance.
Detailed Description
The present application is further described with reference to specific examples.
Example 1
The preparation method of the oil-in-water type high alcohol emulsion comprises the following steps:
1) mixing 25 parts of C18 alcohol (with an acid value of 0.05mg KOH/g), 1 part of C16 alcohol, 1 part of lauric acid and 0.05 part of p-toluenesulfonic acid under the protection of nitrogen, heating to 150 ℃, and preserving heat for 3 hours;
2) cooling the mixture obtained in the step 1) to 100 ℃, adding 0.5 part of nonylphenol polyoxyethylene (20) ether, preserving the temperature and stirring for 30 min;
3) 67.45 parts of water with the temperature of 70 ℃ is slowly added into the mixture obtained in the step 2), and the mixture is kept warm and stirred for 30 min;
4) and (3) cooling the mixture obtained in the step 3) to room temperature through high-speed shearing equipment, and adding 5 parts of polyacrylic acid thickening agent to obtain a product with the viscosity of 1320 mPa.s.
Example 2
The preparation method of the oil-in-water type high alcohol emulsion comprises the following steps:
1) mixing 10 parts of C22 alcohol (the acid value is 1.0mg KOH/g), 5 parts of C12 alcohol, 3 parts of stearic acid and 0.2 part of p-toluenesulfonic acid under the protection of nitrogen, heating to 180 ℃, and preserving heat for 3 hours;
2) cooling the mixture obtained in the step 1) to 90 ℃, adding 5 parts of stearyl alcohol polyoxyethylene (20) ether, preserving heat and stirring for 30 min;
3) slowly adding 76.3 parts of water with the temperature of 100 ℃ into the mixture obtained in the step 2), preserving the temperature and stirring for 30 min;
4) and (4) cooling the mixture obtained in the step 3) to room temperature through high-speed shearing equipment, and adding 0.5 part of hydroxyethyl cellulose thickener to obtain a product with the viscosity of 515 mPa.s.
Example 3
The preparation method of the oil-in-water type high alcohol emulsion comprises the following steps:
1) mixing 15 parts of C18-C26 mixed alcohol (the acid value is 0.5mg KOH/g), 3 parts of C12-C16 mixed alcohol, 2 parts of oleic acid and 0.1 part of concentrated sulfuric acid under the protection of nitrogen, heating to 160 ℃, and preserving heat for 3 hours;
2) cooling the mixture obtained in the step 1) to 95 ℃, adding 3 parts of oleic acid polyoxyethylene (20) ether, preserving heat and stirring for 30 min;
3) slowly adding 73.9 parts of 90 ℃ water into the mixture obtained in the step 2), preserving heat and stirring for 30 min;
4) and (3) passing the mixture obtained in the step 3) through a high-speed shearing device, cooling to room temperature, and adding 3 parts of polyacrylamide thickener to obtain a product with the viscosity of 638 mPa.s.
Comparative example 1
The preparation method of the oil-in-water type high alcohol emulsion comprises the following steps:
1) mixing 25 parts of C18 alcohol (with an acid value of 0.01mg KOH/g), 1 part of C16 alcohol, 1 part of lauric acid and 0.05 part of p-toluenesulfonic acid under the protection of nitrogen, heating to 150 ℃, and preserving heat for 3 hours;
2) cooling the mixture obtained in the step 1) to 100 ℃, adding 0.5 part of nonylphenol polyoxyethylene (20) ether, preserving the temperature and stirring for 30 min;
3) 67.45 parts of water with the temperature of 70 ℃ are slowly added into the mixture obtained in the step 2), and the mixture is kept warm and stirred for 30 min;
4) and (3) cooling the mixture obtained in the step 3) to room temperature through high-speed shearing equipment, and adding 5 parts of polyacrylic acid thickening agent to obtain a product with the viscosity of 1410 mPa.s.
Comparative example 2
The preparation method of the oil-in-water type high alcohol emulsion comprises the following steps:
1) mixing 15 parts of C22 alcohol (the acid value is 1.0mgKOH/g), 3 parts of stearic acid and 0.2 part of p-toluenesulfonic acid under the protection of nitrogen, heating to 180 ℃, and preserving heat for 3 hours;
2) cooling the mixture obtained in the step 1) to 90 ℃, adding 5 parts of stearyl alcohol polyoxyethylene (20) ether, preserving heat and stirring for 30 min;
3) slowly adding 76.3 parts of water with the temperature of 100 ℃ into the mixture obtained in the step 2), preserving the temperature and stirring for 30 min;
4) and (3) cooling the mixture obtained in the step 3) to room temperature through high-speed shearing equipment, and adding 0.5 part of hydroxyethyl cellulose thickener to obtain a product with the viscosity of 852 mPa.s.
Comparative example 3
The preparation method of the oil-in-water type high alcohol emulsion comprises the following steps:
1) mixing 17 parts of C18-C26 mixed alcohol (the acid value is 0.5mgKOH/g) and 3 parts of C12-C16 mixed alcohol, 0.1 part of concentrated sulfuric acid, heating to 160 ℃ under the protection of nitrogen, and preserving heat for 3 hours;
2) cooling the mixture obtained in the step 1) to 95 ℃, adding 3 parts of oleic acid polyoxyethylene (20) ether, preserving heat and stirring for 30 min;
3) slowly adding 73.9 parts of 90 ℃ water into the mixture obtained in the step 2), preserving heat and stirring for 30 min;
4) and (3) passing the mixture obtained in the step 3) through high-speed shearing equipment, cooling to room temperature, and adding 3 parts of polyacrylamide thickener to obtain a product with the viscosity of 476 mPa.s.
Comparative example 4
The preparation method of the oil-in-water type high alcohol emulsion comprises the following steps:
1) heating 10 parts of C22 alcohol (acid value of 1.0mgKOH/g) and 8.2 parts of lauryl stearate to 90 deg.C under stirring, adding 5 parts of stearyl polyoxyethylene (20) ether, maintaining temperature and stirring for 30 min;
2) slowly adding 76.3 parts of water with the temperature of 100 ℃ into the mixture obtained in the step 2), preserving the temperature and stirring for 30 min;
3) and (3) cooling the mixture obtained in the step 3) to room temperature through high-speed shearing equipment, and adding 0.5 part of hydroxyethyl cellulose thickener to obtain a product with the viscosity of 565 mPa.s.
Example 4 Performance testing
The products prepared in the above examples and comparative examples were tested for properties as follows:
1. storage stability test
The product was left at 25 ℃ for 6 months and a follow-up test of viscosity was carried out. The viscosity tester is Brookfield DV2TLV with test conditions of 2# rotor, 6rpm, in mPa.s. Specific results are shown in table 1.
TABLE 1 storage stability test results (unit: mPa. s)
| Product(s) | Initial viscosity | 2 weeks | 1 month | 3 months old | 6 months old |
| Example 1 | 1320 | 1452 | 1415 | 1376 | 1583 |
| Example 2 | 515 | 478 | 576 | 545 | 568 |
| Example 3 | 638 | 634 | 679 | 720 | 683 |
| Comparative example 1 | 1410 | 1540 | 2360 | 4503 | ＞5000 |
| Comparative example 2 | 852 | ＞5000 | - | - | - |
| Comparative example 3 | 476 | 652 | 898 | 2430 | 4620 |
| Comparative example 4 | 565 | 893 | 2543 | ＞5000 | - |
As can be seen from the viscosity tracking results in Table 1, the viscosity of the product prepared in the present application has a small change in viscosity within 6 months, while the viscosity of the product prepared in the comparative example has a significant increase within 6 months.
2. Test for degassing Property
The test is carried out by using an ETG gas content tester, corrugated paper pulp of a certain domestic paper mill is selected, the addition amount of a degassing agent is 5ppm, and the degassing performance at 20 ℃, 40 ℃ and 60 ℃ is respectively tested. The test results are shown in Table 2, and the lower the test value (in%) indicates the better the degassing performance.
TABLE 2 degassing Performance test results (unit:%)
From the test results in Table 2, it can be seen that the products of the examples have better degassing performance at three temperatures of 20 deg.C, 40 deg.C and 60 deg.C, while the products of the comparative examples do not allow for three temperatures.
Claims (9)
1. An oil-in-water type higher alcohol emulsion composition is characterized by comprising the following components in percentage by weight: 10-25% of fatty alcohol with high carbon number, 1-5% of fatty alcohol with low carbon number, 1-3% of fatty acid, 0.05-0.2% of catalyst, 0.5-5% of nonionic surfactant, 0.5-5% of thickening agent and the balance of water; wherein the fatty alcohol with high carbon number is C18-C30 fatty alcohol, and the acid value range is 0.05-1.0mg KOH/g; the fatty alcohol with low carbon number is C12-C16 fatty alcohol; the fatty acid is C12-C22 fatty acid.
2. The oil-in-water type higher alcohol emulsion composition according to claim 1, wherein the higher carbon number fatty alcohol is selected from one or more of mono C18 alcohol, mono C20 alcohol, mono C22 alcohol, mono C24 alcohol, mono C26 alcohol, mono C28 alcohol, mono C30 alcohol, C18-C26 mixed alcohol, C24-C28 mixed alcohol, and C20-C28 mixed alcohol.
3. The oil-in-water type higher alcohol emulsion composition according to claim 1, wherein the lower carbon number fatty alcohol is selected from one or more of mono C12 alcohol, mono C14 alcohol, mono C16 alcohol, C12-C16 mixed alcohol, and C12-C14 mixed alcohol.
4. The oil-in-water high alcohol emulsion composition according to claim 1, wherein the fatty acid is selected from one or more of monolauric acid, myristic acid, palmitic acid, stearic acid, arachidic acid, behenic acid, and oleic acid.
5. The oil-in-water type higher alcohol emulsion composition according to claim 1, wherein the catalyst is one selected from the group consisting of concentrated sulfuric acid, concentrated hydrochloric acid, and p-toluenesulfonic acid.
6. The oil-in-water type higher alcohol emulsion composition according to claim 1, wherein the nonionic surfactant is selected from the group consisting of alkylphenol ethoxylates, fatty alcohol ethoxylates, and fatty acid polyoxyethylene esters.
7. The oil-in-water type higher alcohol emulsion composition according to claim 1 or 6, wherein the nonionic surfactant is selected from the group consisting of polyoxyethylene (20) nonylphenol ether, polyoxyethylene (20) stearyl ether, polyoxyethylene (20) stearate, polyoxyethylene (20) oleate, polyoxyethylene (20) castor oil ether, polyoxyethylene sorbitan monostearate, sorbitan monooleate, sorbitan tristearate, sorbitan trioleate, ethylene glycol stearate, ethylene glycol laurate, propylene glycol oleate, propylene glycol stearate, glycerol monostearate, glycerol monolaurate, diethylene glycol monolaurate, pentaerythritol stearate, polyoxyethylene (20) sorbitan monooleate, polyoxyethylene (20) sorbitan tristearate, polyethylene glycol 4000 monooleate, Polyethylene glycol 2000 monolaurate.
8. The oil-in-water high alcohol emulsion composition according to claim 1, wherein the thickener is selected from the group consisting of hydroxyethyl cellulose, carboxymethyl cellulose, xanthan gum, polyacrylamide, polyacrylic acid.
9. The method for producing an oil-in-water type higher alcohol emulsion according to claim 1, comprising the steps of:
1) mixing and stirring high-carbon fatty alcohol, low-carbon fatty alcohol, fatty acid and a catalyst under the protection of nitrogen, heating to 150 ℃ and 180 ℃, and preserving heat for 3 hours;
2) cooling the mixture obtained in the step 1) to 90-100 ℃, adding an emulsifier, preserving heat and stirring for 30 min;
3) slowly adding water with the temperature of 70-100 ℃ into the mixture obtained in the step 2), preserving heat and stirring for 30 min;
4) and 3) passing the mixture obtained in the step 3) through high-speed shearing equipment, cooling to room temperature, and adding a thickening agent to obtain the target product.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115155115A (en) * | 2022-08-19 | 2022-10-11 | 济宁金汉斯环保材料股份有限公司 | High-carbon alcohol emulsion defoaming agent for papermaking and preparation method and application thereof |
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