CN112111340B - Environment-friendly cleaning agent with low VOCs content - Google Patents
Environment-friendly cleaning agent with low VOCs content Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/28—Organic compounds containing halogen
- C11D7/30—Halogenated hydrocarbons
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/26—Organic compounds containing oxygen
- C11D7/261—Alcohols; Phenols
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/26—Organic compounds containing oxygen
- C11D7/266—Esters or carbonates
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/26—Organic compounds containing oxygen
- C11D7/267—Heterocyclic compounds
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/50—Solvents
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- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Emergency Medicine (AREA)
- Detergent Compositions (AREA)
- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
Abstract
The invention provides an environment-friendly cleaning agent with low VOCs content. The cleaning agent comprises the following raw materials in percentage by mass: n-bromopropane: 10% -60%; solvent oil: 20 to 80 percent; butylene oxide: 1% -5%; alcohol: 1% -40%; a dioxolane: 0% -5%; ethyl acetate: 0 to 5 percent. The cleaning agent belongs to an environment-friendly cleaning agent with low VOCs content, and has the advantages of no damage to an ozone layer, strong cleaning capability, high permeability, difficult combustion, strong stability, no corrosion to precision electronic devices such as semiconductors, low cost, low requirement on cleaning equipment and the like; the cleaning flux shows excellent effect when applied.
Description
Technical Field
The invention relates to an environment-friendly cleaning agent with low VOCs content, belonging to the technical field of cleaning agents.
Background
After the welding of precision electronic devices such as semiconductors and the like is finished, various residues such as soldering flux, oil stains and the like exist on the surfaces of the precision electronic devices; reliability and stability of the semiconductor may be reduced during its use; therefore, the surface of the semiconductor needs to be cleaned before use. The flux is used for the purpose of obtaining sufficient solderability in the soldering process of electronic products in order to remove oxide films on the surfaces of solder and a base material or to prevent reoxidation of the surfaces of the solder and the base material; the flux is corrosive, and the flux remaining on the surface of the base material after soldering may reduce the quality of the finished substrate. The commonly used flux mainly includes rosin flux mainly containing rosin or rosin derivatives, and water-soluble flux mainly containing polyol resins. The common cleaning method is dipping method, dipping shaking method, spraying method, air spraying method, ultrasonic method, etc. The cleaning agent for cleaning precision electronic devices such as semiconductors in the market is mainly organic fluorides, alkyl and brominated alkanes.
The organic fluorides are mainly cleaning agents replacing CFC-113, and mainly include cleaning agents containing HCFC (hydrogen-containing chlorofluorocarbon), HFC (hydrogen-containing fluorocarbon), HFE (hydrofluoroether), PFC (perfluorocarbon), and the like. The cleaning agent has the cleaning performance close to CFC-113, is stable, low in toxicity, non-inflammable, safe and reliable, but is generally expensive. HCFC has certain influence on the ozone layer; HCFC-141B, HCFC-225, a transitional substitute, is used in large quantities and is ultimately forbidden. After the "kyoto protocol" has formally come into effect, the organofluoride-based cleaning agent is at risk of being restricted in use.
The hydrocarbon-based cleaning agent is a cleaning agent containing two elements of carbon and hydrogen, such as TF-2000-1, also called as carbonhydrate or hydrocarbon solvent in Japan, and is widely used. The cleaning agent has the advantages of non-ODS, strong cleaning power to oil stains, good permeability, no taste or slight odor, low toxicity, easy treatment of waste liquid, renewable utilization and low price; the disadvantages are inflammable and explosive, slow drying, high requirement for cleaning equipment, high equipment cost, complex operation and relatively low efficiency.
Brominated alkane cleaning agents are a cleaning agent which is widely used in 2015 in the United states and Japan, and in the fields of electronic industry, aviation industry, automobile industry and household appliances. The bromoalkane cleaning agent mainly comprises n-bromopropane (NPB), the performance of the bromoalkane cleaning agent can be compared with that of CFC-113 and TCA, the main technical parameters are almost the same as that of TCA, the wetting coefficient is better, the cleaning capability for metal parts is stronger, the bromoalkane cleaning agent can be recycled, the use cost is very low, the cleaning process is completely consistent with that of CFC and TCA, equipment does not need to be replaced, only the steaming and washing temperature needs to be adjusted, and the bromoalkane cleaning agent is also called as a 'substitute cleaning agent for the third world'. However, the cleaning agent has high content of VOCs, and is not an environment-friendly cleaning agent.
In order to solve the above problems, patent document CN1445352A discloses a cleaning agent for electronic devices, which is composed of dichloropentafluoropropane and a mixture of alkanes having carbon numbers of 5 to 15. The electronic equipment cleaning agent is low in ozone consumption potential, has moderate dissolving performance and volatilization rate, is suitable for cleaning electronic equipment, and is particularly suitable for cleaning electronic equipment in an operating state or a charged state. Patent document CN1884465A discloses an on-line cleaning agent for precision electronic instruments and a production method thereof, wherein the cleaning agent is composed of dichloropentafluoropropane, trichloroethane and monofluorodichloroethane. The cleaning agent has high cleaning power, no residue, and insulation property of 2.6 × 1012Omega; the cleaning agent has higher voltage resistance, and the voltage resistance value is 25 kv. Although the cleaning agent does not damage the ozone layer, the price of the dioxy-pentafluoropropane on the market is high. Patent document CN106916652A discloses an environment-friendly cleaning agent, which comprises: 94% -95% of n-bromopropane by using amount as a raw material; 3% -4% of n-propanol; 0.2 percent of nitromethane; 0.8% of 1, 3-dioxolane; 0.7 percent of butylene oxide; BHT 0.3%. The cleaning agent has the advantages of low ozone destruction index, low global warming effect, good environmental protection effect, high cleaning effect, high permeability, easy cleaning of microporous materials, high drying speed, no flash point and low hydrolysis degree, but has low boiling point, strong volatility and high VOCs content, and does not belong to an environment-friendly cleaning agent.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides an environment-friendly cleaning agent with low VOCs content. The cleaning agent belongs to an environment-friendly cleaning agent with low VOCs content, and has the advantages of no damage to an ozone layer, strong cleaning capability, high permeability, nonflammability, strong stability, no corrosion to precision electronic devices such as semiconductors, low cost, low requirement on cleaning equipment and the like.
The technical scheme of the invention is as follows:
an environment-friendly cleaning agent with low VOCs content is composed of the following raw materials in percentage by mass:
n-bromopropane: 10 to 60 percent
Solvent oil: 20 to 80 percent
Butylene oxide: 1 to 5 percent
Alcohol: 1 to 40 percent
A dioxolane: 0 to 5 percent
Ethyl acetate: 0 to 5 percent.
According to the invention, the environment-friendly cleaning agent with low VOCs content is preferably prepared from the following raw materials in percentage by mass:
n-bromopropane: 20 to 50 percent
Solvent oil: 30 to 60 percent
Butylene oxide: 1 to 3 percent
Alcohol: 10 to 15 percent
A dioxolane: 0.5 to 3 percent
Ethyl acetate: 0.5 to 4 percent.
Preferably, the environment-friendly cleaning agent with low VOCs content is composed of the following raw materials in percentage by mass:
n-bromopropane: 20 to 50 percent
Solvent oil: 30 to 60 percent
Butylene oxide: 2 to 3 percent of
Alcohol: 10 to 15 percent
A dioxolane: 1.5 to 3 percent
Ethyl acetate: 1.5 to 4 percent.
According to the invention, the boiling point range of the solvent oil is preferably 100-350 ℃; preferably, the solvent oil is one or a combination of more than two of 120# solvent oil, 190# solvent oil, 200# solvent oil, 260# solvent oil, D60 solvent oil, D65 solvent oil or D70 solvent oil.
Preferably, according to the invention, the alcohol is a linear or branched alcohol having from C1 to C10; preferably, the alcohol is one or a combination of two or more of methanol, ethanol, n-propanol, isopropanol, n-butanol, isobutanol, octyl butanol or isopropyl ethanol.
The environment-friendly cleaning agent with low VOCs content is prepared by directly and physically mixing n-bromopropane, solvent oil, butylene oxide, alcohol, dioxolane and ethyl acetate.
The invention has the technical characteristics and beneficial effects that:
(1) the cleaning agent disclosed by the invention uses the n-bromopropane, so that the problems of low flash point and flammability of other cleaning aids (such as solvent oil and the like) are solved.
The hydrocarbon cleaning agent (such as solvent oil) burns to generate a substance capable of reacting with oxygen in the atmosphere and forms H2-O2And the system emits heat.
The combustion reaction is as follows:
·H+O2→·OH+O·
·O+H2→·OH+H·
the main exothermic reactions are as follows:
·OH+CO→CO2+H·
the primary flame retardant effect of n-bromopropane is achieved by a gas phase mechanism; when the cleaning agent is in the initial stage of combustion, the n-bromopropane is thermally decomposed to obtain hydrogen bromide gas, and the hydrogen bromide gas captures high-activity H in the gas phase·And OH·Liberating less active Br·Free radicals, which cause combustion to terminate, have a flame-retardant reaction as follows:
C3H7Br→HBr+C3H6
H·+HBr→H2+Br·
OH·+HBr→H2O+Br·
in conclusion, the use of the n-bromopropane in the cleaning agent enables the cleaning agent to have the characteristics of no flash point and non-flammability, thereby reducing the requirements on cleaning equipment.
(2) The solvent oil is used in the cleaning agent, so that on one hand, the cleaning agent has a cleaning effect in cooperation with other components; on the other hand, the consumption of the n-bromopropane is reduced, so that the cleaning agent disclosed by the invention can meet the standard requirements of GB38508-2020 'limit of content of volatile organic compounds of the cleaning agent' by using common cleaning modes (such as air shower cleaning, ultrasonic cleaning and the like), and belongs to an environment-friendly cleaning agent with low content of VOCs. In addition, the invention avoids the use of organic fluorides and has the advantages of no damage to the ozone layer, low cost and the like.
(3) The alcohol, the dioxolane and the ethyl acetate in the cleaning agent form synergistic cleaning with the n-bromopropane and the solvent oil during azeotropic aerosol cleaning, and the effects of high permeability and strong cleaning capability are realized.
(4) The epoxy butane used in the cleaning agent stabilizes the acid value in the cleaning agent, and achieves the effect of not corroding precision electronic devices such as semiconductors.
The n-bromopropane can decompose hydrogen bromide in the long-term recycling or high-temperature using process, and the epoxybutane reacts with the free hydrogen bromide in the cleaning agent, so that the acid value of the cleaning agent is stabilized, and the specific reaction formula is as follows:
C3H7Br→C3H6+HBr
CH3CH2CHOCH2+HBr→CH3CH2CHOHCH2Br
(5) the cleaning agent disclosed by the invention has an excellent cleaning effect when being applied to cleaning of the soldering flux, can effectively remove the soldering flux, and has strong cleaning capability and high permeability.
Detailed Description
The present invention will be further described with reference to the following examples, but is not limited thereto.
Meanwhile, the experimental methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials are commercially available, unless otherwise specified.
Example 1
An environment-friendly cleaning agent with low VOCs content is composed of the following raw materials by mass:
20kg of n-bromopropane, 60kg of 120# solvent oil, 10kg of n-propanol, 5kg of isopropyl alcohol, 2kg of epoxy butane, 1.5kg of dioxolane and 1.5kg of ethyl acetate.
The raw materials are uniformly mixed to obtain the environment-friendly cleaning agent with flame retardance.
Example 2
An environment-friendly cleaning agent with low VOCs content is composed of the following raw materials by mass:
40kg of n-bromopropane, 40kg of 200# solvent oil, 10kg of isopropanol, 5kg of n-butanol, 2kg of butylene oxide, 1.5kg of dioxolane and 1.5kg of ethyl acetate.
The raw materials are uniformly mixed to obtain the environment-friendly cleaning agent with flame retardance.
Example 3
An environment-friendly cleaning agent with low VOCs content is composed of the following raw materials by mass:
30kg of n-bromopropane, 50kg of No. 260 mineral spirit, 5kg of n-propanol, 10kg of isobutanol, 2kg of butylene oxide, 1.5kg of dioxolane and 1.5kg of ethyl acetate.
The raw materials are uniformly mixed to obtain the environment-friendly cleaning agent with flame retardance.
Example 4
An environment-friendly cleaning agent with low VOCs content is composed of the following raw materials by mass:
50kg of n-bromopropane, 35kg of D60 solvent oil, 5kg of n-propanol, 5kg of isopropanol, 3kg of butylene oxide, 1kg of dioxolane and 1kg of ethyl acetate.
The raw materials are uniformly mixed to obtain the environment-friendly cleaning agent with flame retardance.
Example 5
An environment-friendly cleaning agent with low VOCs content is composed of the following raw materials by mass:
50kg of n-bromopropane, 30kg of D70 solvent oil, 10kg of n-butanol, 3kg of epoxybutane, 3kg of dioxolane and 4kg of ethyl acetate.
The raw materials are uniformly mixed to obtain the environment-friendly cleaning agent with flame retardance.
Comparative example 1
The cleaning agent is composed of the following raw materials by mass:
20kg of n-bromopropane, 10kg of n-propanol, 5kg of isopropyl alcohol, 2kg of epoxybutane, 1.5kg of dioxolane and 1.5kg of ethyl acetate.
And (3) uniformly mixing the raw materials to obtain the cleaning agent.
Comparative example 2
The cleaning agent is composed of the following raw materials by mass:
60kg of No. 120 solvent oil, 10kg of n-propanol, 5kg of isopropyl alcohol, 1.5kg of dioxolane and 1.5kg of ethyl acetate.
And (3) uniformly mixing the raw materials to obtain the cleaning agent.
Comparative example 3
The cleaning agent is composed of the following raw materials by mass:
20kg of n-bromopropane, 60kg of 120# solvent oil, 10kg of n-propanol, 5kg of isopropyl alcohol, 1.5kg of dioxolane and 1.5kg of ethyl acetate.
And (3) uniformly mixing the raw materials to obtain the cleaning agent.
Comparative example 4
The cleaning agent is composed of the following raw materials by mass:
20kg of n-bromopropane, 60kg of 120# solvent oil and 2kg of epoxy butane.
And (3) uniformly mixing the raw materials to obtain the cleaning agent.
Comparative example 5
The cleaning agent is composed of the following raw materials by mass:
95kg of n-bromopropane, 3kg of n-propanol, 0.2kg of nitromethane, 0.7kg of butylene oxide, 0.8kg of dioxolane and 0.3kg of BHT.
And (3) uniformly mixing the raw materials to obtain the cleaning agent.
Test example:
evaluation test 1: content of VOCs
The cleaning agent disclosed by the invention is detected according to the content limit value of the volatile organic compounds of the cleaning agent in the standard GB 38508-.
Evaluation test 2: acidity of the solution
The acidity of the cleaning agent is detected according to an acidity detection method in the enterprise standard QB/0783SXH 001-.
Evaluation test 3: flash point
The test is based on the standard GB/T21929-2008 Tager closed cup flash point measurement method, under the specified test conditions, the sample is caused to flash by using a fire source to be corrected to the lowest temperature under the atmospheric pressure of 101.325kPa (760 mmHg). When a flame appears and instantly spreads to the whole liquid level, the sample is considered to reach the flash point. When a burning source is used as the test flame, the test flame may produce a blue halo or flame augmentation before the true flash point occurs, which is not a flash fire and should be ignored. The results are shown in Table 3.
Evaluation test 4: continuous combustion
According to the standard GB/T21622-2008 method for the continuous combustion test of the flammable liquid of the dangerous goods, the continuous combustion tests are respectively carried out at two temperatures of 60.5 ℃ and 75 ℃. The results are shown in Table 3.
In the context of Table 3, the following examples are,
v: the test specimen continued to burn.
X: the test specimen did not burn continuously.
Evaluation test 5: cleaning performance
Manufacturing a test substrate: a lead-free solder paste was printed on a copper pattern of an epoxy resin copper-clad laminate (50 × 50 × 1.0mm) using a metal mask, and a test board having a flux attached thereto was prepared by reflow soldering under the conditions shown in table 1 below.
Table 1 reflow soldering condition table of test substrates
| Atmosphere(s) | Air (a) |
| Rate of temperature rise | 2℃/s |
| Preheating | 180℃、80s |
| Peak temperature | 260℃、60s |
Cleaning test: the test method was air shower method, and the cleaning conditions are shown in table 2. The cleaning agent with the temperature of 70 ℃ is contacted with the test substrate for 0.5-1 minute for cleaning, then the test substrate is rinsed for 1 minute by flowing deionized water, then the test substrate is blown for 1 minute to remove water for drying, and the cleaning degree of the soldering flux on the surface of the test substrate after drying is judged visually. The results are shown in Table 3.
Table 2 air shower cleaning conditions:
in the context of Table 3, the following examples are,
very good: the flux was removed well for both 0.5 and 1 minute cleaning times (0% surface area of flux residue).
O: under the condition that the cleaning time is 0.5 minute, the soldering flux has residues; however, when the cleaning time was 1 minute, the flux was removed well (the surface area of the flux residue was 0%).
And (delta): in the case of a cleaning time of 1 minute, some flux remains (flux residue surface area greater than 0% and less than 10%).
Table 3 table of performance data of cleaning agents
As can be seen from the data in Table 3, the content of VOCs is obviously reduced by adding the solvent oil into the cleaning agent; because of the presence of the n-bromopropane, the cleaning agent disclosed by the invention has the advantages that the flash point of the cleaning agent is not detected, the cleaning agent does not continuously burn, and the cleaning effect is better; the cleaning agent does not use n-bromopropane, has a low flash point, generates a phenomenon of continuous combustion, and has a common cleaning effect; after the epoxy butane used as a stabilizer is not used, the acid value is obviously increased, and the washing effect is better; no entrainer is used, the main components of the cleaning agent have poor permeability and poor cleaning effect. Compared with cleaning agents containing other components, the cleaning agent has more excellent performance.
Claims (2)
1. The environment-friendly cleaning agent with low VOCs content is characterized by comprising the following raw materials in percentage by mass:
n-bromopropane: 20 to 50 percent
Solvent oil: 30 to 60 percent
Butylene oxide: 1 to 3 percent
Alcohol: 10 to 15 percent
A dioxolane: 0.5 to 3 percent
Ethyl acetate: 0.5% -4%;
the solvent oil is one or the combination of more than two of 120# solvent oil, 190# solvent oil, 200# solvent oil, 260# solvent oil, D60 solvent oil, D65 solvent oil or D70 solvent oil; the alcohol is one or the combination of more than two of normal propyl alcohol, isopropyl alcohol, normal butyl alcohol or isobutyl alcohol.
2. The environment-friendly cleaning agent with low content of VOCs according to claim 1, which is characterized by comprising the following raw materials in percentage by mass:
n-bromopropane: 20 to 50 percent
Solvent oil: 30 to 60 percent
Butylene oxide: 2 to 3 percent
Alcohol: 10 to 15 percent
A dioxolane: 1.5 to 3 percent
Ethyl acetate: 1.5% -4%.
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| JP2004018789A (en) * | 2002-06-19 | 2004-01-22 | Mihama Kk | Detergent composition for dry cleaning |
| CN101942366A (en) * | 2010-03-10 | 2011-01-12 | 江西瑞思博化工有限公司 | Electrical equipment cleaning agent |
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| CN106811341A (en) * | 2015-11-30 | 2017-06-09 | 周子童 | Environment-friendly cleaning agent |
| CN106916652A (en) * | 2015-12-28 | 2017-07-04 | 天津市绿通环保工程设备开发有限公司 | Environment-friendly cleaning agent |
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| JP2004018789A (en) * | 2002-06-19 | 2004-01-22 | Mihama Kk | Detergent composition for dry cleaning |
| CN101942366A (en) * | 2010-03-10 | 2011-01-12 | 江西瑞思博化工有限公司 | Electrical equipment cleaning agent |
| CN102504972A (en) * | 2011-11-18 | 2012-06-20 | 天津博克尼科技发展有限公司 | Cleaning agent for welding agent on circuit board of computer |
| CN106811341A (en) * | 2015-11-30 | 2017-06-09 | 周子童 | Environment-friendly cleaning agent |
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Address after: 262714 Shouguang Yangkou Chemical Industrial Park, Weifang City, Shandong Province (West of Yanglin road and north of Donghai Road) Patentee after: Shandong XURUI New Material Co.,Ltd. Patentee after: Shandong Green Marine Chemical Industry Research Institute Co., Ltd Address before: 262714 Bohai Industrial Park, Yangkou Town, Shouguang City, Weifang City, Shandong Province Patentee before: SHANDONG SUNRIS CO.,LTD. Patentee before: Shandong Green Marine Chemical Industry Research Institute Co., Ltd |