CN112010773A - Dehydrating agent and preparation method thereof, and hydrocarbon water cutting agent and preparation method thereof - Google Patents
Dehydrating agent and preparation method thereof, and hydrocarbon water cutting agent and preparation method thereof Download PDFInfo
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- CN112010773A CN112010773A CN202010841099.3A CN202010841099A CN112010773A CN 112010773 A CN112010773 A CN 112010773A CN 202010841099 A CN202010841099 A CN 202010841099A CN 112010773 A CN112010773 A CN 112010773A
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- dehydrating agent
- dehydrating
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C231/00—Preparation of carboxylic acid amides
- C07C231/02—Preparation of carboxylic acid amides from carboxylic acids or from esters, anhydrides, or halides thereof by reaction with ammonia or amines
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C233/00—Carboxylic acid amides
- C07C233/01—Carboxylic acid amides having carbon atoms of carboxamide groups bound to hydrogen atoms or to acyclic carbon atoms
- C07C233/02—Carboxylic acid amides having carbon atoms of carboxamide groups bound to hydrogen atoms or to acyclic carbon atoms having nitrogen atoms of carboxamide groups bound to hydrogen atoms or to carbon atoms of unsubstituted hydrocarbon radicals
- C07C233/04—Carboxylic acid amides having carbon atoms of carboxamide groups bound to hydrogen atoms or to acyclic carbon atoms having nitrogen atoms of carboxamide groups bound to hydrogen atoms or to carbon atoms of unsubstituted hydrocarbon radicals with carbon atoms of carboxamide groups bound to acyclic carbon atoms of an acyclic saturated carbon skeleton
- C07C233/05—Carboxylic acid amides having carbon atoms of carboxamide groups bound to hydrogen atoms or to acyclic carbon atoms having nitrogen atoms of carboxamide groups bound to hydrogen atoms or to carbon atoms of unsubstituted hydrocarbon radicals with carbon atoms of carboxamide groups bound to acyclic carbon atoms of an acyclic saturated carbon skeleton having the nitrogen atoms of the carboxamide groups bound to hydrogen atoms or to acyclic carbon atoms
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/34—Pretreatment of metallic surfaces to be electroplated
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Electrochemistry (AREA)
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a dehydrating agent and a preparation method thereof, and a hydrocarbon water cutting agent and a preparation method thereof, and relates to the technical field of chemical cleaning. Wherein the dehydrating agent comprises the following components in percentage by mass: 60-80% of an alcohol ether solvent, 5-10% of a phase transfer catalyst, 10-20% of long-chain primary amine and 5-15% of short-chain carboxylic acid. The dehydrating agent provided by the invention has good dehydrating effect and higher efficiency, and the adsorption film on the surface of the part can prevent the part from condensing moisture and adsorbing dust, so that the dehydrating agent can be widely used for the electroplating pretreatment of the part, thereby ensuring the subsequent electroplating effect.
Description
Technical Field
The invention relates to the technical field of chemical cleaning, in particular to a dehydrating agent and a preparation method thereof, and a hydrocarbon water cutting agent and a preparation method thereof.
Background
In the field of electronic elements with higher and higher requirements on material requirements and processing precision, the requirements on surface electroplating of precise hardware parts are also stricter, and the surface cleanliness in the traditional sense cannot meet the processing requirements, so that the cleanliness of a molecular level higher than the traditional requirements is required to meet the surface electroplating conditions with nanometer-level requirements so as to meet the high-precision specification and high-performance reliability of the electronic elements. Therefore, water stains cannot remain on the cleaned parts, and the cleaned parts have certain anti-wetting capability and surface static electricity capability for preventing dust adhesion, otherwise, the electroplating effect is influenced.
Therefore, some enterprises have started to perform dehydration treatment of parts before plating using a dehydrating agent. However, the conventional dehydrating agents generally have problems of long treatment time and poor dehydrating effect.
Disclosure of Invention
The invention mainly aims to provide a dehydrating agent and a preparation method thereof, and a hydrocarbon water cutting agent and a preparation method thereof, and aims to provide a dehydrating agent with high efficiency and good dehydrating effect.
In order to achieve the purpose, the invention provides a dehydrating agent which comprises the following components in percentage by mass:
60-80% of an alcohol ether solvent, 5-10% of a phase transfer catalyst, 10-20% of long-chain primary amine and 5-15% of short-chain carboxylic acid.
Optionally, the alcohol ether solvent comprises at least one of ethylene glycol tert-butyl ether, dimethyl propylene glycol methyl ether, and diethylene glycol butyl ether.
Optionally, the phase transfer catalyst comprises at least one of methyltrioctylammonium chloride, methyldioctylammonium chloride, and methyltrisononyl ammonium chloride.
Optionally, the long-chain primary amine comprises at least one of dodecylamine, tetradecylamine, hexadecylamine, and octadecylamine.
Optionally, the short chain carboxylic acid comprises at least one of hexanoic acid, heptanoic acid, octanoic acid, and nonanoic acid.
The invention also provides a preparation method of the dehydrating agent, which comprises the following steps:
and (3) uniformly mixing the alcohol ether solvent, the phase transfer catalyst, the long-chain primary amine and the short-chain carboxylic acid, and reacting for 20-30 min at 23-27 ℃ to obtain the dehydrating agent.
The invention also provides a hydrocarbon water cutting agent, which comprises the following components in percentage by mass:
97-99.6% of hydrocarbon solvent and 0.4-3% of dehydrating agent;
wherein the dehydrating agent is the dehydrating agent as described above.
Optionally, the hydrocarbon solvent comprises at least one of normal alkanes with 9-11 carbon atoms.
In addition, the invention also provides a preparation method of the hydrocarbon water cutting agent, which comprises the following steps:
and mixing and stirring the dehydrating agent and the hydrocarbon solvent uniformly to obtain the hydrocarbon water cutting agent.
According to the technical scheme provided by the invention, long-chain primary amine and short-chain carboxylic acid are quickly generated into the amide compound through the phase transfer catalyst, the amide group on the amide compound forms a molecular adsorption film on the surface of the part to be treated, the long-chain group on the amide compound forms an extremely strong hydrophobic layer, and along with the generation of the adsorption film, moisture on the surface of the part is squeezed by the hydrophobic layer formed by the long-chain group and quickly falls in a bead shape.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
In the field of electronic elements with higher and higher requirements on material requirements and processing precision, the requirements on surface electroplating of precise hardware parts are also stricter, the parts need to be cleaned before electroplating, water stains can not be left on the cleaned parts, certain wetting resistance and surface static electricity capability for preventing dust adhesion are required, and the electroplating effect is influenced otherwise. Therefore, some enterprises have started to perform dehydration treatment of parts before plating using a dehydrating agent. However, the conventional dehydrating agents generally have problems of long treatment time and poor dehydrating effect.
In view of the above, the invention provides a dehydrating agent, which comprises the following components in percentage by mass:
60-80% of an alcohol ether solvent, 5-10% of a phase transfer catalyst, 10-20% of long-chain primary amine and 5-15% of short-chain carboxylic acid.
According to the technical scheme provided by the invention, long-chain primary amine and short-chain carboxylic acid are quickly generated into the amide compound through the phase transfer catalyst, the amide group on the amide compound forms a molecular adsorption film on the surface of the part to be treated, the long-chain group on the amide compound forms an extremely strong hydrophobic layer, and along with the generation of the adsorption film, moisture on the surface of the part is squeezed by the hydrophobic layer formed by the long-chain group and quickly falls in a bead shape.
The alcohol ether solvent comprises at least one of ethylene glycol tert-butyl ether, dimethyl propylene glycol methyl ether and diethylene glycol butyl ether. The alcohol ether solvent can be one or more of ethylene glycol tert-butyl ether, dimethyl propylene glycol methyl ether and diethylene glycol butyl ether.
The phase transfer catalyst comprises at least one of methyl trioctyl ammonium chloride, methyl dioctyl ammonium chloride and methyl trinonyl ammonium chloride. Phase transfer catalysts are a class of catalysts that can help transfer reactants from one phase to another phase where the reaction can occur, thereby accelerating the reaction rate of a heterogeneous system. In the embodiment, the long-chain primary amine and the short-chain carboxylic acid are quickly generated into the amide compound through the phase transfer catalyst, so that the prepared dehydrating agent can be quickly dehydrated, and the dehydrating efficiency is improved.
The long-chain primary amine comprises at least one of dodecylamine, tetradecylamine, hexadecylamine and octadecylamine.
The short chain carboxylic acid comprises at least one of hexanoic acid, heptanoic acid, octanoic acid, and nonanoic acid. The short-chain carboxylic acid is used for reacting with long-chain primary amine to generate an amide compound, the amide group on the amide compound can form a molecular adsorption film on the surface of the part, but the adsorption film does not form a complete film at once, in the generation process of the adsorption film, the long-chain group at the N end of the amide compound forms a hydrophobic layer to separate moisture on the surface of the part from the part, after the part is gradually coated by the adsorption film, the moisture on the part is completely separated, and the adsorption film enables the part to be difficult to condense moisture and adsorb dust.
The invention also provides a preparation method of the dehydrating agent, which comprises the following steps:
and (3) uniformly mixing the alcohol ether solvent, the phase transfer catalyst, the long-chain primary amine and the short-chain carboxylic acid, and reacting for 20-30 min at 23-27 ℃ to obtain the dehydrating agent.
The invention does not limit the charging sequence of the alcohol ether solvent, the phase transfer catalyst, the long-chain primary amine and the short-chain carboxylic acid, preferably, the alcohol ether solvent is firstly added, then the phase transfer catalyst is added, the long-chain primary amine and the short-chain carboxylic acid are sequentially added after stirring and dissolving, and the charging sequence ensures that the color, the state, the effect and the stability of the hydrocarbon water cutting agent finally prepared by the dehydrating agent are better.
By improving the components and the proportion of the dehydrating agent, the preparation time of the dehydrating agent is shorter, the preparation condition is mild, and the time and the cost are saved; meanwhile, in the production process, the material can be fed at one time, the situation that different types of functional materials are added in multiple steps to achieve a composite effect is avoided, and safety accidents such as leakage, splashing and the like are easily caused when the materials are added in multiple steps is avoided, so that the requirements on the operation safety in the production process are particularly high, the cost is higher, and the safety of operators is not facilitated. In conclusion, the preparation method of the dehydrating agent saves time and cost, and is safe and convenient to operate.
The specific use mode of the dehydrating agent is not limited, and the dehydrating agent can be mixed with an organic solvent according to a certain volume ratio to obtain a water cutting agent, and then the parts to be treated are put into the water cutting agent to be dehydrated successfully. Preferably, the organic solvent is a hydrocarbon solvent, so the invention further provides a hydrocarbon water cutting agent, which comprises the following components in percentage by mass: 97-99.6% of hydrocarbon solvent and 0.4-3% of dehydrating agent.
The hydrocarbon solvent comprises at least one of n-alkanes with 9-11 carbon atoms. Namely, the hydrocarbon solvent comprises one or more of a mixture of n-alkane with nine carbon atoms, n-alkane with ten carbon atoms and n-alkane with eleven carbon atoms.
When the prepared hydrocarbon water cutting agent is used, parts to be treated are slowly placed into the environment-friendly hydrocarbon water cutting agent, standing is carried out for 5s, water films on the surfaces of the parts quickly fall on a lower hydrocarbon layer in a bead shape, then the parts are slowly pulled up and placed for 2-5 minutes until the parts are completely volatilized, the parts can be packaged and shipped to the next procedure, the requirements of conditions such as temperature and the like do not exist during use, the operation is convenient, and the efficiency is high.
Further, the invention also provides a preparation method of the hydrocarbon water cutting agent, which comprises the following steps:
and adding a hydrocarbon solvent into the dehydrating agent, and uniformly stirring to obtain the hydrocarbon water cutting agent.
After the hydrocarbon water cutting agent prepared by the invention is generated, the property is stable, the transportation, the split charging and the use are facilitated, and the practicability is higher.
The technical solutions of the present invention are further described in detail with reference to the following specific examples, which should be understood as merely illustrative and not limitative.
Example 1
(1) Weighing the following raw materials: 33.25g of dimethyl propylene glycol methyl ether (66.5%), 3.5g of methyl trioctyl ammonium chloride (7%), 7.25g of dodecylamine (14.5%), 6g of octanoic acid (12%).
(2) Adding dimethyl propylene glycol methyl ether into a reaction kettle, adding methyl trioctyl ammonium chloride, stirring for dissolving, sequentially adding dodecylamine and caprylic acid, stirring for reacting for 30min at 25 ℃, and generating a transparent reaction product N- (dodecyl) octylamide, namely a dehydrating agent.
Example 2
(1) Weighing the following raw materials: 30g of ethylene glycol tert-butyl ether (60%), 2.5g of methyltrioctylammonium chloride (5%), 5g of tetradecylamine (10%), 7.5g of hexanoic acid (15%).
(2) Adding ethylene glycol tert-butyl ether into a reaction kettle, adding methyl trioctyl ammonium chloride, stirring for dissolving, adding tetradecylamine and hexanoic acid, stirring for reacting for 25min at the temperature of 27 ℃, and generating a transparent reaction product N- (tetradecyl) hexylamide, namely a dehydrating agent.
Example 3
(1) Weighing the following raw materials: 30g of a mixture of dimethylpropanediol methyl ether and diethylene glycol butyl ether (60%), 5g of a mixture of methyltrioctylammonium chloride and methyldioctylammonium chloride (10%), 10g of hexadecylamine (20%), 5g of heptanoic acid (10%).
(2) Adding a mixture of dimethyl propylene glycol methyl ether and diethylene glycol butyl ether, a mixture of methyl trioctyl ammonium chloride and methyl dioctyl ammonium chloride, hexadecylamine and heptanoic acid into a reaction kettle, uniformly mixing, and stirring and reacting at 25 ℃ for 20min to generate a reaction product, namely a dehydrating agent.
Example 4
(1) Weighing the following raw materials: 40g of ethylene glycol tert-butyl ether, a mixture of dimethyl propylene glycol methyl ether and diethylene glycol butyl ether (80%), 2.5g of methyl trinonyl ammonium chloride (5%), 5g of a mixture of lauryl and stearyl amines (10%), 2.5g of a mixture of caprylic and pelargonic acids (5%).
(2) Adding a mixture of ethylene glycol tert-butyl ether, dimethyl propylene glycol methyl ether and diethylene glycol butyl ether into a reaction kettle, adding methyl trinonyl ammonium chloride, stirring and dissolving, sequentially adding a mixture of dodecylamine and octadecylamine and a mixture of octanoic acid and pelargonic acid, and stirring and reacting at 23 ℃ for 30min to generate a reaction product, namely a dehydrating agent.
Example 5
10g of the dehydrating agent (2%) prepared in example 1 was added to a reaction kettle, and 490g of n-decaalkane (98%) was added thereto, and the mixture was stirred uniformly until it was transparent, i.e., a hydrocarbon water-cutting agent.
Example 6
8g of the dehydrating agent (0.4%) prepared in example 2 was charged into a reaction vessel, and 1992g of n-nonadecane (99.6%) was added thereto, and the mixture was stirred until it was transparent, i.e., a hydrocarbon water-cutting agent.
Example 7
10g of the dehydrating agent (2%) prepared in example 3 was added to a reaction kettle, and 490g of n-decadecane (98%) was added and stirred uniformly to obtain a hydrocarbon water cutting agent.
Example 8
9g of the dehydrating agent (3%) prepared in example 4 was added to a reaction kettle, and 291g of a mixture (97%) of n-decadecane and n-undecane was added thereto, and the mixture was stirred uniformly to obtain a hydrocarbon water-cutting agent.
5 same-batch materials of SUS316 in a signal shielding case inside a mobile phone are punched and polished, a series of water-based cleaning agents are used for removing wax, tap water and pure water are used for rinsing for three times respectively to serve as parts to be treated, then the hydrocarbon water cutting agent prepared in the embodiments 5 to 8 is treated, and an existing 1145W water cutting agent (which can be prepared by the company, the production reaction time of the preparation is 1-2 hours, and the reaction temperature is 70-90 ℃) of a certain company is used as a comparative example for treating the SUS316, and the treatment method and the results are as follows:
5 parts to be treated are respectively and slowly put into the water cutting agents of the examples and the comparative examples, the parts are kept stand, then the parts are slowly pulled up and placed until the volatilization is complete (namely the drying time), the parts can be packaged and shipped to the next procedure, and the parameters and the performance test results in the treatment process are shown in the table 1.
Table 1 testing of parameters and performance of water-cutting agent during use
According to the method, when the hydrocarbon water cutting agent is prepared, the time required by the production reaction is 20-30 min, the temperature required by the reaction is 23-27 ℃, and when the water cutting agent in the comparative example is prepared, the time required by the production reaction is 1-2 h, and the temperature required by the reaction is 70-90 ℃, so that the preparation time of the dehydrating agent is shorter, the reaction condition is mild, the time and the cost are saved, and the time and the cost of the finally prepared hydrocarbon water cutting agent are saved. Meanwhile, as can be seen from table 1, the dehydration time of the hydrocarbon water cutting agent prepared by the method only needs 5s, while the comparative example needs 1min, and the dehydration defective rate and the electroplating defective rate are both lower than the comparative example.
In conclusion, the hydrocarbon water cutting agent provided by the invention can save time and cost during preparation, the prepared hydrocarbon water cutting agent has higher dehydration speed and good dehydration effect, and parts treated by the hydrocarbon water cutting agent are beneficial to ensuring the subsequent electroplating effect, so that the hydrocarbon water cutting agent has obvious advantages compared with the existing water cutting agent.
The above is only a preferred embodiment of the present invention, and it is not intended to limit the scope of the invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention shall be included in the scope of the present invention.
Claims (9)
1. The dehydrating agent is characterized by comprising the following components in percentage by mass:
60-80% of an alcohol ether solvent, 5-10% of a phase transfer catalyst, 10-20% of long-chain primary amine and 5-15% of short-chain carboxylic acid.
2. The dehydrating agent according to claim 1, wherein the alcohol ether solvent comprises at least one of ethylene glycol t-butyl ether, dimethyl propylene glycol methyl ether and diethylene glycol butyl ether.
3. The dehydrating agent according to claim 1, wherein the phase transfer catalyst comprises at least one of methyltrioctylammonium chloride, methyldioctylammonium chloride, and methyltrisonylammonium chloride.
4. The dehydrating agent according to claim 1, wherein the long-chain primary amine comprises at least one of dodecylamine, tetradecylamine, hexadecylamine, and octadecylamine.
5. The dehydrating agent according to claim 1, wherein the short-chain carboxylic acid comprises at least one of caproic acid, heptanoic acid, caprylic acid and nonanoic acid.
6. A method for preparing a dehydrating solvent according to any one of claims 1 to 5, comprising the steps of:
and (3) uniformly mixing the alcohol ether solvent, the phase transfer catalyst, the long-chain primary amine and the short-chain carboxylic acid, and reacting for 20-30 min at 23-27 ℃ to obtain the dehydrating agent.
7. The hydrocarbon water cutting agent is characterized by comprising the following components in percentage by mass:
97-99.6% of hydrocarbon solvent and 0.4-3% of dehydrating agent;
wherein the dehydrating agent is the dehydrating agent according to any one of claims 1 to 5.
8. The hydrocarbon water cutting agent according to claim 7, wherein the hydrocarbon solvent comprises at least one of n-alkanes having 9 to 11 carbon atoms.
9. A method for preparing the hydrocarbon water-cutting agent as claimed in claim 7 or 8, characterized by comprising the steps of:
and mixing and stirring the dehydrating agent and the hydrocarbon solvent uniformly to obtain the hydrocarbon water cutting agent.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010841099.3A CN112010773A (en) | 2020-08-18 | 2020-08-18 | Dehydrating agent and preparation method thereof, and hydrocarbon water cutting agent and preparation method thereof |
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| CN202010841099.3A CN112010773A (en) | 2020-08-18 | 2020-08-18 | Dehydrating agent and preparation method thereof, and hydrocarbon water cutting agent and preparation method thereof |
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Cited By (2)
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| CN114134548A (en) * | 2021-12-07 | 2022-03-04 | 安美科技股份有限公司 | Hydrocarbon water cutting agent and preparation process thereof |
| EP4105301A1 (en) * | 2021-06-15 | 2022-12-21 | Basf Se | New gasoline additive packages |
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