CN113121844A - Preparation method of nanoscale emulsified wax - Google Patents
Preparation method of nanoscale emulsified wax Download PDFInfo
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- CN113121844A CN113121844A CN201911420971.0A CN201911420971A CN113121844A CN 113121844 A CN113121844 A CN 113121844A CN 201911420971 A CN201911420971 A CN 201911420971A CN 113121844 A CN113121844 A CN 113121844A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/26—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers modified by chemical after-treatment
- C08J2323/30—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers modified by chemical after-treatment by oxidation
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Abstract
The invention discloses a preparation method of nanoscale emulsifying wax, which adopts the following raw materials in parts by weight: 150 parts of deionized water, 9-15 parts of fatty alcohol-polyoxyethylene ether, 40 parts of low-density oxidized polyethylene wax, 0.5-1.5 parts of potassium hydroxide, 0.1-0.5 part of sodium sulfite and 0.5 part of preservative. In the aspect of production quality, materials in one reaction kettle are uniform, so that the problem of non-uniformity caused by adding firstly and then adding when two reaction kettles are operated is solved; from the safety perspective, one reaction kettle is easier to control, two reaction kettles are easy to cause poor matching, and the two reaction kettles are lost to cause safety problems, in addition, the whole operation is carried out under normal pressure, and the possibility of explosion is avoided; from the product angle, the appearance of the product is in a slightly sticky and transparent state, the emulsion particle size is finer, more uniform and more stable, and the storage time can be prolonged.
Description
Technical Field
The invention relates to the field of fine chemical engineering, in particular to a preparation method of nanoscale emulsifying wax.
Background
OPE (oxidized polyethylene) wax is low molecular weight polyethylene containing hydroxyl groups and carboxyl groups. The high-temperature-stability high-temperature-volatility white yellowish powder has the special properties of low viscosity, high softening point, good hardness and the like, is non-toxic, good in thermal stability, low in high-temperature volatility, white and slightly yellowish, and has good chemical stability. OPE cannot be directly dissolved in water, and needs to be dissolved in water to form an emulsion through a certain production method. The oxidized polyethylene wax emulsion can be used in a large number of aqueous coating and ink formulations, providing excellent rub, stick, and scratch resistance. It can also be used as raw and auxiliary materials for textile softening agent, car wax and leather softening agent.
Generally, the product with the average particle size of less than 500nm is called wax emulsion, and the product with the average particle size of less than 100nm is called microemulsion; products with an average particle size of more than 500nm are called wax dispersions, whereas products with a particle size of less than 1 μm are called microdispersions.
The oxidized polyethylene wax emulsion on the market at present has a large particle diameter of about 0.1-0.5 micrometer (mum), is milky in appearance, affects luster after coating, is easy to delaminate and agglomerate in an actual storage stage, has a storage time as short as 6 months, and affects storage and use.
Disclosure of Invention
The present invention aims to overcome the above-mentioned shortcomings and provide a technical solution to solve the above-mentioned problems.
A preparation method of nanoscale emulsifying wax adopts the following raw materials in parts by weight: 150 parts of deionized water, 9-15 parts of fatty alcohol-polyoxyethylene ether, 40 parts of low-density oxidized polyethylene wax, 0.5-1.5 parts of potassium hydroxide, 0.1-0.5 part of sodium sulfite and 0.5 part of preservative;
the nanoscale emulsifying wax is prepared by the following steps:
the method comprises the following steps: adding deionized water, fatty alcohol-polyoxyethylene ether and low-density oxidized polyethylene wax into a reaction kettle, stirring, heating and mixing, heating to 100-102 ℃, preserving heat and standing after heating is finished to obtain a mixed solution;
step two: adding potassium hydroxide into the mixed solution, stirring and mixing, and then keeping the temperature and standing to obtain a secondary mixed solution;
step three: adding sodium sulfite into the secondary mixed solution, stirring and mixing again, and then keeping the temperature and standing for 5-10 min to obtain a tertiary mixed solution;
step four: and (3) detecting the third mixed solution, if the third mixed solution is transparent, cooling, reducing the temperature to below 40 ℃, adding a preservative, mixing and stirring, cooling to normal temperature to obtain nanoscale emulsified wax, taking out and packaging.
Compared with the prior art, the invention has the beneficial effects that: the invention has simple processing steps and low processing cost.
In terms of yield, one reaction kettle is used for production, no loss is caused, and all added materials can be fully utilized;
in the aspect of production quality, materials in one reaction kettle are uniform, so that the problem of non-uniformity caused by adding firstly and then adding when two reaction kettles are operated is solved;
on the energy efficiency, the energy consumption is saved by 35% when one reaction kettle is heated compared with two reaction kettles;
from the safety perspective, one reaction kettle is easier to control, two reaction kettles are easy to cause poor matching, and the two reaction kettles are lost to cause safety problems, in addition, the whole operation is carried out under normal pressure, and the possibility of explosion is avoided;
from the perspective of environmental protection, one reaction kettle is almost free of any discharge, and water for cleaning the reaction kettle can be recycled when secondary production occurs;
from the product angle, the appearance of the product is in a slightly sticky and transparent state, the emulsion particle size is finer, more uniform and more stable, and the storage time can be prolonged.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the embodiment of the invention, the preparation method of the nanoscale emulsified wax adopts the following raw materials in parts by weight: 150 parts of deionized water, 9-15 parts of fatty alcohol-polyoxyethylene ether, 40 parts of low-density oxidized polyethylene wax, 0.5-1.5 parts of potassium hydroxide, 0.1-0.5 part of sodium sulfite and 0.5 part of preservative;
the nanoscale emulsifying wax is prepared by the following steps:
the method comprises the following steps: adding deionized water, fatty alcohol-polyoxyethylene ether and low-density oxidized polyethylene wax into a reaction kettle, stirring, heating and mixing, heating to 100-102 ℃, preserving heat and standing after heating is finished to obtain a mixed solution;
step two: adding potassium hydroxide into the mixed solution, stirring and mixing, and then keeping the temperature and standing to obtain a secondary mixed solution;
step three: adding sodium sulfite into the secondary mixed solution, stirring and mixing again, and then keeping the temperature and standing for 5-10 min to obtain a tertiary mixed solution;
step four: and (3) detecting the third mixed solution, if the third mixed solution is transparent, cooling, reducing the temperature to below 40 ℃, adding a preservative, mixing and stirring, cooling to normal temperature to obtain nanoscale emulsified wax, taking out and packaging.
2. The method for preparing nano-sized emulsifying wax according to claim 1, wherein the time for standing under heat preservation in the first step is 5min to 20 min.
3. The method for preparing nano-sized emulsifying wax according to claim 1, wherein the stirring speed in the first step is 10 to 35 r/min.
4. The method for preparing nano-sized emulsifying wax according to claim 1, wherein the time for standing under heat preservation in the second step is 5min to 10 min.
5. The method for preparing nanometer emulsified wax as claimed in claim 1, wherein the time for standing under heat preservation in step three is 5min to 10 min.
[ EXAMPLES one ]
A preparation method of nanoscale emulsifying wax adopts the following raw materials in parts by weight: 150 parts of deionized water, 9 parts of fatty alcohol-polyoxyethylene ether, 40 parts of low-density oxidized polyethylene wax, 0.5 part of potassium hydroxide, 0.1 part of sodium sulfite and 0.5 part of preservative;
the nanoscale emulsifying wax is prepared by the following steps:
the method comprises the following steps: adding deionized water, fatty alcohol-polyoxyethylene ether and low-density oxidized polyethylene wax into a reaction kettle, stirring, heating and mixing, heating to 100-102 ℃, preserving heat and standing after heating is finished to obtain a mixed solution;
step two: adding potassium hydroxide into the mixed solution, stirring and mixing, and then keeping the temperature and standing to obtain a secondary mixed solution;
step three: adding sodium sulfite into the secondary mixed solution, stirring and mixing again, and then keeping the temperature and standing for 5-10 min to obtain a tertiary mixed solution;
step four: and (3) detecting the third mixed solution, if the third mixed solution is transparent, cooling, reducing the temperature to below 40 ℃, adding a preservative, mixing and stirring, cooling to normal temperature to obtain nanoscale emulsified wax, taking out and packaging.
[ example two ]
A preparation method of nanoscale emulsifying wax adopts the following raw materials in parts by weight: 150 parts of deionized water, 12 parts of fatty alcohol-polyoxyethylene ether, 40 parts of low-density oxidized polyethylene wax, 1 part of potassium hydroxide, 0.3 part of sodium sulfite and 0.5 part of preservative;
the nanoscale emulsifying wax is prepared by the following steps:
the method comprises the following steps: adding deionized water, fatty alcohol-polyoxyethylene ether and low-density oxidized polyethylene wax into a reaction kettle, stirring, heating and mixing, heating to 100-102 ℃, preserving heat and standing after heating is finished to obtain a mixed solution;
step two: adding potassium hydroxide into the mixed solution, stirring and mixing, and then keeping the temperature and standing to obtain a secondary mixed solution;
step three: adding sodium sulfite into the secondary mixed solution, stirring and mixing again, and then keeping the temperature and standing for 5-10 min to obtain a tertiary mixed solution;
step four: and (3) detecting the third mixed solution, if the third mixed solution is transparent, cooling, reducing the temperature to below 40 ℃, adding a preservative, mixing and stirring, cooling to normal temperature to obtain nanoscale emulsified wax, taking out and packaging.
[ EXAMPLE III ]
A preparation method of nanoscale emulsifying wax adopts the following raw materials in parts by weight: 150 parts of deionized water, 15 parts of fatty alcohol-polyoxyethylene ether, 40 parts of low-density oxidized polyethylene wax, 1.5 parts of potassium hydroxide, 0.5 part of sodium sulfite and 0.5 part of preservative;
the nanoscale emulsifying wax is prepared by the following steps:
the method comprises the following steps: adding deionized water, fatty alcohol-polyoxyethylene ether and low-density oxidized polyethylene wax into a reaction kettle, stirring, heating and mixing, heating to 100-102 ℃, preserving heat and standing after heating is finished to obtain a mixed solution;
step two: adding potassium hydroxide into the mixed solution, stirring and mixing, and then keeping the temperature and standing to obtain a secondary mixed solution;
step three: adding sodium sulfite into the secondary mixed solution, stirring and mixing again, and then keeping the temperature and standing for 5-10 min to obtain a tertiary mixed solution;
step four: and (3) detecting the third mixed solution, if the third mixed solution is transparent, cooling, reducing the temperature to below 40 ℃, adding a preservative, mixing and stirring, cooling to normal temperature to obtain nanoscale emulsified wax, taking out and packaging.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Claims (8)
1. The preparation method of the nanoscale emulsified wax is characterized by adopting the following raw materials in parts by weight: 150 parts of deionized water, 9-15 parts of fatty alcohol-polyoxyethylene ether, 40 parts of low-density oxidized polyethylene wax, 0.5-1.5 parts of potassium hydroxide, 0.1-0.5 part of sodium sulfite and 0.5 part of preservative;
the nanoscale emulsifying wax is prepared by the following steps:
the method comprises the following steps: adding deionized water, fatty alcohol-polyoxyethylene ether and low-density oxidized polyethylene wax into a reaction kettle, stirring, heating and mixing, heating to 100-102 ℃, preserving heat and standing after heating is finished to obtain a mixed solution;
step two: adding potassium hydroxide into the mixed solution, stirring and mixing, and then keeping the temperature and standing to obtain a secondary mixed solution;
step three: adding sodium sulfite into the secondary mixed solution, stirring and mixing again, and then keeping the temperature and standing for 5-10 min to obtain a tertiary mixed solution;
step four: and (3) detecting the third mixed solution, if the third mixed solution is transparent, cooling, reducing the temperature to below 40 ℃, adding a preservative, mixing and stirring, cooling to normal temperature to obtain nanoscale emulsified wax, taking out and packaging.
2. The method for preparing nano-sized emulsifying wax according to claim 1, wherein the time for standing under heat preservation in the first step is 5min to 20 min.
3. The method for preparing nano-sized emulsifying wax according to claim 1, wherein the stirring speed in the first step is 10 to 35 r/min.
4. The method for preparing nano-sized emulsifying wax according to claim 1, wherein the time for standing under heat preservation in the second step is 5min to 10 min.
5. The method for preparing nanometer emulsified wax as claimed in claim 1, wherein the time for standing under heat preservation in step three is 5min to 10 min.
6. The method for preparing nano-emulsified wax according to claim 1, wherein the following raw materials are used in weight ratio: 150 parts of deionized water, 9 parts of fatty alcohol-polyoxyethylene ether, 40 parts of low-density oxidized polyethylene wax, 0.5 part of potassium hydroxide, 0.1 part of sodium sulfite and 0.5 part of preservative.
7. The method for preparing nano-emulsified wax according to claim 1, wherein the following raw materials are used in weight ratio: 150 parts of deionized water, 12 parts of fatty alcohol-polyoxyethylene ether, 40 parts of low-density oxidized polyethylene wax, 1 part of potassium hydroxide, 0.3 part of sodium sulfite and 0.5 part of preservative.
8. The method for preparing nano-emulsified wax according to claim 1, wherein the following raw materials are used in weight ratio: 150 parts of deionized water, 15 parts of fatty alcohol-polyoxyethylene ether, 40 parts of low-density oxidized polyethylene wax, 1.5 parts of potassium hydroxide, 0.5 part of sodium sulfite and 0.5 part of preservative.
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Citations (7)
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CN101289540A (en) * | 2008-06-12 | 2008-10-22 | 广东纺织职业技术学院 | Method for preparing oxidic polyethylene wax microemulsion |
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CN102827378A (en) * | 2012-09-21 | 2012-12-19 | 南京天诗新材料科技有限公司 | Method for continuously preparing wax emulsion |
CN103696262A (en) * | 2013-12-20 | 2014-04-02 | 中山时进纺织原料有限公司 | Preparation method of anti-run smoothing agent for fabrics |
CN103755978A (en) * | 2014-01-13 | 2014-04-30 | 广东工业大学 | Preparation method of oxidized polyethylene wax emulsion |
CN103865186A (en) * | 2012-12-12 | 2014-06-18 | 上海雅运纺织助剂有限公司 | Oxidized polyethylene wax micro-emulsion composition and preparation method thereof |
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2019
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CN101942152A (en) * | 2009-07-06 | 2011-01-12 | 上海雅运纺织助剂有限公司 | Microemulsion composite of polyethylene wax oxide |
CN102190801A (en) * | 2011-03-29 | 2011-09-21 | 湖南科技大学 | Preparation method for nonionic oxidized polyethylene wax emulsion using single emulsifier |
CN102827378A (en) * | 2012-09-21 | 2012-12-19 | 南京天诗新材料科技有限公司 | Method for continuously preparing wax emulsion |
CN103865186A (en) * | 2012-12-12 | 2014-06-18 | 上海雅运纺织助剂有限公司 | Oxidized polyethylene wax micro-emulsion composition and preparation method thereof |
CN103696262A (en) * | 2013-12-20 | 2014-04-02 | 中山时进纺织原料有限公司 | Preparation method of anti-run smoothing agent for fabrics |
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