CN113528248B - Hydrocarbon cleaning agent for semiconductor and preparation method - Google Patents

Hydrocarbon cleaning agent for semiconductor and preparation method Download PDF

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CN113528248B
CN113528248B CN202110849480.9A CN202110849480A CN113528248B CN 113528248 B CN113528248 B CN 113528248B CN 202110849480 A CN202110849480 A CN 202110849480A CN 113528248 B CN113528248 B CN 113528248B
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hydrocarbon
mixed solution
cleaning agent
solvent
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CN113528248A (en
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吴爱平
郝光磊
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Rema Environmental Protection Technology Jiangsu Co ltd
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    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/66Non-ionic compounds
    • C11D1/72Ethers of polyoxyalkylene glycols
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/66Non-ionic compounds
    • C11D1/825Mixtures of compounds all of which are non-ionic
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/66Non-ionic compounds
    • C11D1/83Mixtures of non-ionic with anionic compounds
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    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16Organic compounds
    • C11D3/18Hydrocarbons
    • C11D3/181Hydrocarbons linear
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    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16Organic compounds
    • C11D3/20Organic compounds containing oxygen
    • C11D3/2068Ethers
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    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16Organic compounds
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    • C11D3/245Organic compounds containing halogen containing fluorine
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    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16Organic compounds
    • C11D3/36Organic compounds containing phosphorus
    • C11D3/361Phosphonates, phosphinates or phosphonites
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    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
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    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/43Solvents
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    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/02Anionic compounds
    • C11D1/12Sulfonic acids or sulfuric acid esters; Salts thereof
    • C11D1/14Sulfonic acids or sulfuric acid esters; Salts thereof derived from aliphatic hydrocarbons or mono-alcohols
    • C11D1/146Sulfuric acid esters
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    • C11D1/00Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/66Non-ionic compounds
    • C11D1/667Neutral esters, e.g. sorbitan esters
    • C11D2111/22

Abstract

The application relates to the field of semiconductor cleaning agents, and particularly discloses a hydrocarbon cleaning agent for a semiconductor and a preparation method thereof. The hydrocarbon cleaning agent is prepared from the following raw materials in parts by weight: 40-80 parts of hydrocarbon solvent, 10-60 parts of alcohol ether solvent, 1-5 parts of fine particle remover, 0.1-10 parts of scaling powder remover, 0.5-5 parts of anti-whitening agent and 0.1-5 parts of surface tension auxiliary agent; the preparation method comprises the following steps: s1, weighing a hydrocarbon solvent, an alcohol ether solvent, a fine particle remover, a scaling powder remover, a whitening inhibitor and a surface tension auxiliary agent according to parts by weight; s2, uniformly mixing a hydrocarbon solvent and an alcohol ether solvent to prepare a mixed solution A; s3, uniformly mixing the fine particle remover, the soldering flux remover, the anti-whitening agent and the surface tension auxiliary agent to prepare a mixed solution B; s4, pouring the mixed solution B into the mixed solution A, and uniformly stirring to obtain a mixed solution C; s5, standing the mixed liquid C, and preparing a hydrocarbon cleaning agent finished product after the mixed liquid C is stable. The hydrocarbon cleaning agent has the advantage of low VOCs content.

Description

Hydrocarbon cleaning agent for semiconductor and preparation method
Technical Field
The application relates to the technical field of semiconductor cleaning agents, in particular to a hydrocarbon cleaning agent for a semiconductor and a preparation method thereof.
Background
The semiconductor refers to a material with electric conductivity between a conductor and an insulator at normal temperature, and is applied to the fields of integrated circuits, consumer electronics, communication systems, photovoltaic power generation, illumination, high-power conversion and the like. In order to ensure the quality and high reliability of the semiconductor device, the semiconductor device needs to be cleaned before packaging. The semiconductor cleaning agent is mainly used for cleaning paraffin, grease and grease macromolecular compounds stained on the surface, metal atoms and metal ions stained on the surface and the like.
Because of the environmental protection requirement and the regulation of 'limit of volatile organic content of cleaning agent' (GB38508-2020), the semiconductor solvent type cleaning agent commonly used in the market at present is generally halogenated hydrocarbon or 141B or a mixture of several kinds of halogenated hydrocarbon and 141B, and the content of VOCs of the cleaning agent is more than 1000g/L and exceeds the upper limit of GB38508-2020, so that the semiconductor cleaning agent with low content of VOCs is required to be provided.
Disclosure of Invention
In order to reduce volatile organic compounds of the semiconductor cleaning agent, the application provides a hydrocarbon cleaning agent of a semiconductor and a preparation method thereof.
In a first aspect, the present application provides a hydrocarbon cleaning agent for semiconductors, which adopts the following technical scheme:
a hydrocarbon cleaning agent for semiconductors is prepared from the following raw materials in parts by weight: 40-80 parts of hydrocarbon solvent, 10-60 parts of alcohol ether solvent, 1-5 parts of fine particle remover, 0.1-10 parts of soldering flux remover, 0.5-5 parts of anti-whitening agent and 0.1-5 parts of surface tension assistant.
By adopting the technical scheme, the hydrocarbon cleaning agent prepared by taking the hydrocarbon solvent as the main agent has the advantages of less evaporation loss, no toxicity, good compatibility with materials, complete volatilization and the like. In addition, the hydrocarbon cleaning agent can be naturally degraded, the cleaning waste liquid can be recycled after distillation, and the air is not polluted. The hydrocarbon cleaning agent does not contain chlorine, and the damage coefficient to ozone is zero. The hydrocarbon cleaning agent prepared by the formula has the VOCs content of less than 800g/L and has excellent environmental protection characteristic.
The cleaning agent also adopts the compounding of the alcohol ether solvent and the hydrocarbon solvent, the hydrocarbon solvent has excellent cleaning performance on non-polar dirt, and the alcohol ether solvent has higher surface activity compared with the hydrocarbon solvent, so that the cleaning agent is used for making up the defect that the cleaning performance of the hydrocarbon solvent on the polar dirt is poor, and the alcohol ether solvent and the hydrocarbon solvent have good synergistic cooperation effect, thereby being beneficial to improving the permeability and the cleaning performance of the hydrocarbon cleaning agent.
Preferably, the hydrocarbon solvent can be one or more of nonane, decane and undecane.
By adopting the technical scheme, the flash points of the nonane, the decane and the undecane are higher, the alkane with the higher flash point is lower in flammability, and the nonane, the decane and the undecane are selected to be used as the hydrocarbon solvent, so that the flammability of the hydrocarbon cleaning agent is favorably reduced.
Preferably, the alcohol ether solvent may be one or more of 3-butoxy-1-propanol, 1-butoxy-2-propanol, 2-tert-butoxyethanol, 3-methoxy-3-methyl-1-butanol.
By adopting the technical scheme, one or more of 3-butoxy-1-propanol, 1-butoxy-2-propanol, 2-tert-butoxyethanol and 3-methoxy-3-methyl-1-butanol are selected as the alcohol ether solvent of the application, mainly for the following three reasons: one is that the components have good compatibility and compatibility with hydrocarbon solvents; secondly, the components have good cooperativity and intermiscibility; and thirdly, the components are cheap and easily available, safe and nontoxic, and have good environmental protection characteristics and low volatility.
Preferably, the fine particle remover may be one or more of HFC-4310mee, HFO-1336mzzZ, 3M7100, 3M 7200.
By adopting the technical scheme, HFC-4310mee, HFO-1336mzzZ, 3M7100 and 3M7200 are all fluorinated liquid, and the fluorinated liquid is selected as the fine particle remover, on one hand, the fluorinated liquid has good cleaning capability of dirt such as metal and the like, and on the other hand, the fluorinated liquid has certain surface activity, and after one or more of the three components are mixed with a hydrocarbon solvent and an alcohol ether solvent, the synergistic effect is good, so that the permeability and the cleaning capability of the hydrocarbon cleaning agent are further improved.
Preferably, the soldering flux remover can be one or a mixture of 365AZ-M and 365 AZ-HM.
By adopting the technical scheme, the 365AZ-M and 365AZ-HM not only have good soldering flux cleaning effect, but also have higher cleaning capability of the dirt on the surfaces of the semiconductor such as resin, oil stain, adhesive and the like, and after one or two of the 365AZ-M and the 365AZ-HM are added into the system, the cleaning range of the hydrocarbon cleaning agent is favorably expanded and the cleaning performance of the hydrocarbon cleaning agent is enhanced.
Preferably, the whitening inhibitor may be diethylene glycol butyl ether.
Through adopting above-mentioned technical scheme, diethylene glycol butyl ether has higher boiling point and lower volatilization rate, has good intermiscibility with the carbon hydrogen solvent in the system, and its dangerization is lower, has good environmental protection characteristic, consequently chooses diethylene glycol butyl ether to use as the whitening preventive of this application.
Preferably, the surface tension auxiliary agent can be one or more of fatty alcohol polyoxyethylene ether, isomeric alcohol polyoxyethylene ether and alkylphenol polyoxyethylene ether.
By adopting the technical scheme, the fatty alcohol-polyoxyethylene ether, the isomeric alcohol-polyoxyethylene ether and the alkylphenol polyoxyethylene ether are all nonionic surfactants, the molecular structures of the three components all contain hydroxyl, the existence of the hydroxyl is favorable for further enhancing the performance of polyether for improving the surface activity of a system, and in addition, the three components and a hydrocarbon solvent have good synergistic effect, so that one or more of the fatty alcohol-polyoxyethylene ether, the isomeric alcohol-polyoxyethylene ether and the alkylphenol polyoxyethylene ether are selected to be used as the surface tension auxiliary agent.
Preferably, the raw material also comprises 0.1-1.5 parts of fatty alcohol ether sodium sulfate and 0.2-2.4 parts of triethanolamine oleate.
By adopting the technical scheme, the fatty alcohol ether sodium sulfate and the triethanolamine oleate are both anionic surfactants, have good intermiscibility with an alcohol ether solvent, have excellent synergistic interaction with the surface tension auxiliary agent, and are beneficial to enhancing the cleaning performance of the hydrocarbon cleaning agent.
Preferably, the raw materials also comprise 1-3 parts of triethyl phosphate and 3-5 parts of diethyl ethylphosphonate.
By adopting the technical scheme, the triethyl phosphate, the ethyl diethyl phosphonate, the hydrocarbon solvent and the alcohol ether solvent have good intermiscibility and compatibility, and the triethyl phosphate and the ethyl diethyl phosphonate have higher flash points, so that the whole flash points of the hydrocarbon cleaning agent are favorably improved, and the flammability risk of the hydrocarbon cleaning agent is reduced. In addition, the triethyl phosphate and the diethyl ethylphosphonate have good flame retardant property, and the flame retardant property of the triethyl phosphate and the diethyl ethylphosphonate is favorably improved when the triethyl phosphate and the diethyl ethylphosphonate are added into a hydrocarbon cleaning agent system. The triethyl phosphate and the diethyl ethylphosphonate also have a synergistic effect, and the combination of the triethyl phosphate and the diethyl ethylphosphonate is favorable for improving the flame retardant effect.
In a second aspect, the application provides a preparation method of a hydrocarbon cleaning agent for semiconductors, which adopts the following technical scheme:
a preparation method of a hydrocarbon cleaning agent for semiconductors comprises the following steps:
s1, weighing a hydrocarbon solvent, an alcohol ether solvent, a fine particle remover, a scaling powder remover, a whitening inhibitor and a surface tension auxiliary agent according to parts by weight;
s2, uniformly mixing a hydrocarbon solvent and an alcohol ether solvent to prepare a mixed solution A;
s3, uniformly mixing the fine particle remover, the soldering flux remover, the anti-whitening agent and the surface tension auxiliary agent to prepare a mixed solution B;
s4, pouring the mixed solution B into the mixed solution A, and uniformly stirring to obtain a mixed solution C;
s5, standing the mixed liquid C, and preparing a hydrocarbon cleaning agent finished product after the mixed liquid C is stable.
By adopting the technical scheme, the hydrocarbon solvent and the alcohol ether solvent are uniformly mixed, the fine particle remover, the scaling powder remover, the whitening preventive and the surface tension auxiliary agent are uniformly mixed, and the mixed liquid B is poured into the mixed liquid A and uniformly stirred to prepare the mixed liquid C, so that the mixing uniformity is improved, the stability of the prepared hydrocarbon cleaning agent is improved, and the generation of flocculate is reduced or even eliminated.
In summary, the present application has the following beneficial effects:
1. because this application adopts hydrocarbon solvent to prepare hydrocarbon cleaner as the main agent for hydrocarbon cleaner has evaporation loss few, nontoxic, good and thoroughly advantages such as volatilizing with the material compatibility. The prepared hydrocarbon cleaning agent has the VOCs content of less than 800g/L and has excellent environmental protection characteristic.
2. In the application, one or more of nonane, decane and undecane are preferably used as hydrocarbon solvents, the nonane, decane and undecane have high flash points, and the alkane with the high flash point has low flammability, so that the flammability of the hydrocarbon cleaning agent is reduced.
3. In the present application, one or more of 3-butoxy-1-propanol, 1-butoxy-2-propanol, 2-t-butoxyethanol, and 3-methoxy-3-methyl-1-butanol are preferably used as the alcohol ether solvent, and the effect of enhancing the effect of the alcohol ether solvent is obtained.
4. The fatty alcohol ether sodium sulfate and the triethanolamine oleate are preferably compounded in the application, have good intermiscibility with the alcohol ether solvent, have excellent synergistic interaction with the surface tension auxiliary agent, and are beneficial to enhancing the cleaning performance of the hydrocarbon cleaning agent.
5. Preferably adopt triethyl phosphate and diethyl ethylphosphonate to compound in this application, both all have good intermiscibility and compatibility with hydrocarbon solvent and alcohol ether solvent, and triethyl phosphate and diethyl ethylphosphonate can improve hydrocarbon cleaner's whole flash point to reduce hydrocarbon cleaner's flammable risk. In addition, the triethyl phosphate and the diethyl ethylphosphonate have good flame retardant performance, and the flame retardant performance of the triethyl phosphate and the diethyl ethylphosphonate can be improved by adding the triethyl phosphate and the diethyl ethylphosphonate into a hydrocarbon cleaning agent system.
Detailed Description
The raw materials used in the application are all purchased from the market.
The present application will be described in further detail with reference to examples.
Examples
Example 1
A hydrocarbon cleaning agent for semiconductors is prepared from the following raw materials in parts by weight: 40kg of nonane, 10kg of 3-butoxy-1-propanol, 1kg of HFC-4310mee, 0.1kg of 365AZ-M, 0.5kg of diethylene glycol monobutyl ether and 0.1kg of fatty alcohol polyoxyethylene ether.
The preparation method of the hydrocarbon cleaning agent for the semiconductor specifically comprises the following steps:
s1, weighing 40kg of nonane, 10kg of 3-butoxy-1-propanol, 1kg of HFC-4310mee, 365AZ-M0.1kg of diethylene glycol monobutyl ether, 0.5kg of diethylene glycol monobutyl ether and 0.1kg of fatty alcohol polyoxyethylene ether;
s2, uniformly mixing nonane and 3-butoxy-1-propanol at normal temperature to prepare a mixed solution A;
s3, uniformly mixing HFC-4310mee, 365AZ-M, diethylene glycol monobutyl ether and fatty alcohol-polyoxyethylene ether at normal temperature to prepare a mixed solution B;
s4, pouring the mixed solution B into the mixed solution A at normal temperature, and uniformly stirring to obtain a mixed solution C;
and S5, standing the mixed solution C at normal temperature, and obtaining a hydrocarbon cleaning agent finished product after the mixed solution C is stabilized.
Example 2
A hydrocarbon cleaning agent for semiconductors is prepared from the following raw materials in parts by weight: 60kg of nonane, 35kg of 3-butoxy-1-propanol, 3kg of HFC-4310mee, 5.2kg of 365AZ-M, 2.75kg of diethylene glycol monobutyl ether and 2.55kg of fatty alcohol polyoxyethylene ether.
The preparation method of the hydrocarbon cleaning agent for the semiconductor specifically comprises the following steps:
s1, weighing 60kg of nonane, 35kg of 3-butoxy-1-propanol, 3kg of HFC-4310mee, 365AZ-M5.2kg of diethylene glycol monobutyl ether and 2.55kg of fatty alcohol polyoxyethylene ether;
s2, uniformly mixing nonane and 3-butoxy-1-propanol at normal temperature to prepare a mixed solution A;
s3, uniformly mixing HFC-4310mee, 365AZ-M, diethylene glycol monobutyl ether and fatty alcohol-polyoxyethylene ether at normal temperature to prepare a mixed solution B;
s4, pouring the mixed solution B into the mixed solution A at normal temperature, and uniformly stirring to obtain a mixed solution C;
and S5, standing the mixed solution C at normal temperature, and obtaining a hydrocarbon cleaning agent finished product after the mixed solution C is stabilized.
Example 3
A hydrocarbon cleaning agent for semiconductors is prepared from the following raw materials in parts by weight: 80kg of nonane, 60kg of 3-butoxy-1-propanol, 5kg of HFC-4310mee, 10kg of 365AZ-M, 5kg of diethylene glycol monobutyl ether and 5kg of fatty alcohol-polyoxyethylene ether.
The preparation method of the hydrocarbon cleaning agent for the semiconductor specifically comprises the following steps:
s1, weighing 80kg of nonane, 60kg of 3-butoxy-1-propanol, 5kg of HFC-4310mee, 365AZ-M10kg, 5kg of diethylene glycol monobutyl ether and 5kg of fatty alcohol polyoxyethylene ether;
s2, uniformly mixing nonane and 3-butoxy-1-propanol at normal temperature to prepare a mixed solution A;
s3, uniformly mixing HFC-4310mee, 365AZ-M, diethylene glycol butyl ether and fatty alcohol polyoxyethylene ether at normal temperature to prepare a mixed solution B;
s4, pouring the mixed solution B into the mixed solution A at normal temperature, and uniformly stirring to obtain a mixed solution C;
and S5, standing the mixed solution C at normal temperature, and obtaining a hydrocarbon cleaning agent finished product after the mixed solution C is stabilized.
Example 4
A hydrocarbon cleaning agent for semiconductors is prepared from the following raw materials in parts by weight: 50kg of decane, 20kg of 1-butoxy-2-propanol, 2kg of HFO-1336mzzZ, 3.5kg of 365AZ-HM, 2kg of diethylene glycol butyl ether and 2kg of isomeric alcohol polyoxyethylene ether.
The preparation method of the hydrocarbon cleaning agent for the semiconductor specifically comprises the following steps:
s1, weighing 50kg of decane, 20kg of 1-butoxy-2-propanol, 2kg of HFO-1336mzzZ, 3.5kg of 365AZ-HM, 2kg of diethylene glycol monobutyl ether and 2kg of isomeric alcohol polyoxyethylene ether;
s2, at normal temperature, uniformly mixing decane and 1-butoxy-2-propanol to prepare a mixed solution A;
s3, preparing mixed liquor B from HFO-1336mzzZ, 365AZ-HM, diethylene glycol monobutyl ether and isomeric alcohol polyoxyethylene ether at normal temperature;
s4, pouring the mixed solution B into the mixed solution A at normal temperature, and uniformly stirring to obtain a mixed solution C;
and S5, standing the mixed solution C at normal temperature, and obtaining a hydrocarbon cleaning agent finished product after the mixed solution C is stabilized.
Example 5
A hydrocarbon cleaning agent for semiconductors is prepared from the following raw materials in parts by weight: 60kg of undecane, 50kg of 2-tert-butoxyethanol, 3M71004kg, 8kg of 365AZ-M and 365AZ-HM with the mass ratio of 1:1, 4kg of diethylene glycol monobutyl ether and 4kg of alkylphenol polyoxyethylene ether.
The preparation method of the hydrocarbon cleaning agent for the semiconductor specifically comprises the following steps:
s1, weighing 60kg of undecane, 50kg of 2-tert-butoxyethanol, 3M71004kg, 365AZ-M and 365AZ-HM8kg in a mass ratio of 1:1, 4kg of diethylene glycol monobutyl ether and 4kg of alkylphenol polyoxyethylene ether;
s2, at normal temperature, uniformly mixing undecane and 2-tert-butoxyethanol to prepare a mixed solution A;
s3, uniformly mixing 3M7100, 365AZ-M and 365AZ-HM in a mass ratio of 1:1, diethylene glycol butyl ether and alkylphenol polyoxyethylene to prepare a mixed solution B at normal temperature;
s4, pouring the mixed solution B into the mixed solution A at normal temperature, and uniformly stirring to obtain a mixed solution C;
and S5, standing the mixed solution C at normal temperature, and obtaining a hydrocarbon cleaning agent finished product after the mixed solution C is stabilized.
Example 6
A hydrocarbon cleaning agent for semiconductors is prepared from the following raw materials in parts by weight: 60kg of nonane and decane with the mass ratio of 1:2, 40kg of 3-methoxy-3-methyl-1-butanol, 3kg of HFC-4310mee and HFO-1336mzzZ with the mass ratio of 1:1, 5kg of 365AZ-M, 2.5kg of diethylene glycol monobutyl ether and 2.5kg of fatty alcohol polyoxyethylene ether and isomeric alcohol polyoxyethylene ether with the mass ratio of 1: 1.
The preparation method of the hydrocarbon cleaning agent for the semiconductor specifically comprises the following steps:
s1, weighing 60kg of nonane and decane, 40kg of 3-methoxy-3-methyl-1-butanol, 3kg of HFC-4310mee and HFO-1336mzzZ in a mass ratio of 1:1, 5kg of 365AZ-M, 2.5kg of diethylene glycol monobutyl ether and 2.5kg of fatty alcohol polyoxyethylene ether and isomeric alcohol polyoxyethylene ether in a mass ratio of 1: 1;
s2, uniformly mixing nonane, decane and 3-methoxy-3-methyl-1-butanol at normal temperature to obtain a mixed solution A;
s3, uniformly mixing HFC-4310mee, HFO-1336mzzZ, 365AZ-M, diethylene glycol butyl ether fatty alcohol polyoxyethylene ether and isomeric alcohol polyoxyethylene ether at normal temperature to prepare a mixed solution B;
s4, pouring the mixed solution B into the mixed solution A at normal temperature, and uniformly stirring to obtain a mixed solution C;
and S5, standing the mixed solution C at normal temperature, and preparing a hydrocarbon cleaning agent finished product after the mixed solution C is stabilized.
Example 7
A hydrocarbon cleaning agent for semiconductors is prepared from the following raw materials in parts by weight: 70kg of decane and undecane with the mass ratio of 1:1, 50kg of 1-butoxy-2-propanol and 2-tert-butoxy ethanol with the mass ratio of 1:2, 5kg of HFO-1336mzzZ and 3M 72004 kg, 365AZ-HM8kg and diethylene glycol monobutyl ether with the mass ratio of 1:1, and 4kg of isomeric alcohol polyoxyethylene ether and alkylphenol polyoxyethylene ether with the mass ratio of 1: 1.
The preparation method of the hydrocarbon cleaning agent for the semiconductor specifically comprises the following steps:
s1, weighing 70kg of decane and undecane in a mass ratio of 1:1, 50kg of 1-butoxy-2-propanol and 2-tert-butoxy ethanol in a mass ratio of 1:2, 5kg of diethylene glycol monobutyl ether and 4kg of isomeric alcohol polyoxyethylene ether and alkylphenol polyoxyethylene ether in a mass ratio of 1:1, wherein the HFO-1336 mzzZZ and 3M 72004 kg are in a mass ratio of 1:1, and 365AZ-HM8kg and the diethylene glycol monobutyl ether are in a mass ratio of 1: 1;
s2, at normal temperature, uniformly mixing decane, undecane, 1-butoxy-2-propanol and 2-tert-butoxy ethanol to obtain a mixed solution A;
s3, at normal temperature, uniformly mixing HFO-1336mzzZ, 3M7200, 365AZ-HM, diethylene glycol butyl ether, isomeric alcohol polyoxyethylene ether and alkylphenol polyoxyethylene ether to prepare a mixed solution B;
s4, pouring the mixed solution B into the mixed solution A at normal temperature, and uniformly stirring to obtain a mixed solution C;
and S5, standing the mixed solution C at normal temperature, and obtaining a hydrocarbon cleaning agent finished product after the mixed solution C is stabilized.
Example 8
A hydrocarbon cleaning agent for semiconductors is prepared from the following raw materials in parts by weight: 50kg of decane, 45kg of 3-butoxy-1-propanol, 1-butoxy-2-propanol and 2-tert-butoxy ethanol in a mass ratio of 1:1:1, 4.5kg of HFC-4310mee and HFO-1336mzzZ in a mass ratio of 1:1, 365AZ-HM7kg, 4kg of diethylene glycol monobutyl ether and 3kg of isomeric alcohol polyoxyethylene ether.
The preparation method of the hydrocarbon cleaning agent for the semiconductor specifically comprises the following steps:
s1, weighing 50kg of decane, 45kg of 3-butoxy-1-propanol, 1-butoxy-2-propanol and 2-tert-butoxy ethanol in a mass ratio of 1:1:1, 4.5kg of HFC-4310mee and HFO-1336mzzZ in a mass ratio of 1:1, 7kg of 365AZ-HM, 4kg of diethylene glycol monobutyl ether and 3kg of isomeric alcohol polyoxyethylene ether;
s2, at normal temperature, uniformly mixing decane, 3-butoxy-1-propanol, 1-butoxy-2-propanol and 2-tert-butoxy ethanol to prepare a mixed solution A;
s3, uniformly mixing HFC-4310mee, HFO-1336mzzZ, 365AZ-HM, diethylene glycol butyl ether and isomeric alcohol polyoxyethylene ether at normal temperature to prepare a mixed solution B;
s4, pouring the mixed solution B into the mixed solution A at normal temperature, and uniformly stirring to obtain a mixed solution C;
and S5, standing the mixed solution C at normal temperature, and obtaining a hydrocarbon cleaning agent finished product after the mixed solution C is stabilized.
Example 9, this example differs from example 8 in that:
the raw material also comprises 0.1 part of fatty alcohol ether sodium sulfate and 0.2 part of triethanolamine oleate.
Example 10, this example differs from example 8 in that:
the raw materials also comprise 0.8 part of fatty alcohol ether sodium sulfate and 1.3 parts of triethanolamine oleate.
Example 11, this example differs from example 8 in that:
the raw materials also comprise 1.5 parts of fatty alcohol ether sodium sulfate and 2.4 parts of triethanolamine oleate.
Example 12, this example differs from example 10 in that:
the raw materials also comprise 1 part of triethyl phosphate and 5 parts of diethyl ethylphosphonate.
Example 13, this example differs from example 10 in that:
the raw materials also comprise 2 parts of triethyl phosphate and 4 parts of diethyl ethylphosphonate.
Example 14, this example differs from example 10 in that:
the raw materials also comprise 3 parts of triethyl phosphate and 3 parts of diethyl ethylphosphonate.
Comparative examples
Comparative example 1, this comparative example differs from example 10 in that:
the raw material also comprises 0.8 part of fatty alcohol ether sodium sulfate.
Comparative example 2, this comparative example differs from example 10 in that:
the raw material also comprises 1.3 parts of triethanolamine oleate.
Comparative example 3, this comparative example differs from example 13 in that:
the raw material also comprises 2 parts of triethyl phosphate.
Comparative example 4, this comparative example differs from example 13 in that:
the raw materials also comprise 4 parts of diethyl ethylphosphonate.
Comparative example
Comparative example 1, which differs from example 2 in that:
nonane was replaced by ethylsiloxane.
Comparative example 2, which differs from example 2 in that:
nonane was replaced by pure water.
Comparative example 3, which differs from example 2 in that:
3-butoxy-1-propanol was deleted.
Performance test
The hydrocarbon cleaning agents prepared in examples 1 to 14, comparative examples 1 to 4 and comparative examples 1 to 3 were sampled, and the samples were subjected to the following performance test tests.
Test method
The VOCs values of the samples were determined according to GB 38508-2020.
The samples were tested for flash point according to GB/T261-2008.
The samples were tested for net wash according to Q/12NK 5119-2012.
The sample is submitted to toxicity testing for toxicity.
The results of the tests are reported in table 1.
TABLE 1
Figure BDA0003181878830000131
Figure BDA0003181878830000141
As can be seen by combining examples 1 to 8 and table 1, examples 1 to 8 are different combinations of the components within the range of the formulation of the hydrocarbon cleaning agent of the present application, and the hydrocarbon cleaning agents prepared by the formulations of examples 1 to 8 all have VOCs meeting emission standards, higher flash points, superior detergency and non-toxicity and environmental protection properties, so that the hydrocarbon cleaning agent prepared by the formulation of the present application has superior non-flammability, detergency and environmental protection properties.
As can be seen by combining examples 1-8 and comparative examples 1-2 with Table 1, the use of a silane organic solvent instead of a hydrocarbon solvent in comparative example 1 resulted in VOCs values in excess of 1000g/L, discharge standards were not met, and the detergency of the cleaning agent was reduced. Compared with the comparative example 1, the cleaning force of the cleaning agent is obviously reduced by adopting pure water to replace a hydrocarbon solvent in the comparative example 2, so that the hydrocarbon cleaning agent has higher cleaning force, and volatile organic compounds meet the national emission standard.
It can be seen from the combination of examples 8 to 11 and table 1 that the detergent cleaning ability of the hydrocarbon cleaning agent prepared by adding the sodium sulfate fatty alcohol ether and the triethanolamine oleate to the system is significantly increased, because the sodium sulfate fatty alcohol ether, the triethanolamine oleate and the surface tension assistant have excellent synergistic effect, which is beneficial to enhancing the cleaning performance of the hydrocarbon cleaning agent.
By combining examples 9-11 and comparative examples 1-2 and table 1, it can be seen that although the addition of the sodium fatty alcohol ether sulfate or the triethanolamine oleate alone has a certain promotion effect on the improvement of the detergency of the hydrocarbon cleaning agent, the improvement performance of the combination of the sodium fatty alcohol ether sulfate and the triethanolamine oleate is more remarkable, which indicates that the sodium fatty alcohol ether sulfate and the triethanolamine oleate have a good synergistic effect.
By combining example 8 and examples 12 to 14 with table 1, it can be seen that the flash point of the hydrocarbon cleaning agent prepared by adding triethyl phosphate and diethyl ethylphosphonate into the system is significantly increased, because both triethyl phosphate and diethyl ethylphosphonate have higher flash points and good flame retardant properties, and the addition of triethyl phosphate and diethyl ethylphosphonate into the hydrocarbon cleaning agent system is beneficial to improving the flame retardant properties.
It can be seen by combining examples 12-14 and comparative examples 3-4 with table 1 that the flash point of the hydrocarbon cleaning agent is also obviously improved by adding triethyl phosphate or diethyl ethylphosphonate alone, but because triethyl phosphate and diethyl ethylphosphonate also have a synergistic effect, the combination of the two is more favorable for improving the flame retardant effect of the hydrocarbon cleaning agent, and therefore, the flash point of the hydrocarbon cleaning agent is increased more significantly when the triethyl phosphate and the diethyl ethylphosphonate are added simultaneously.
In summary, the hydrocarbon cleaning agent for semiconductors in the present application has low VOCs, good non-flammability, excellent cleaning power and low volatility, and can be reused.
The specific embodiments are only for explaining the present application and are not limiting to the present application, and those skilled in the art can make modifications to the embodiments without inventive contribution as required after reading the present specification, but all the embodiments are protected by patent law within the scope of the claims of the present application.

Claims (4)

1. A hydrocarbon cleaning agent for semiconductors is characterized in that: comprises the following raw materials in parts by weight: 40-80 parts of hydrocarbon solvent, 10-60 parts of alcohol ether solvent, 1-5 parts of fine particle remover, 0.1-10 parts of soldering flux remover, 0.5-5 parts of anti-whitening agent and 0.1-5 parts of surface tension assistant;
the hydrocarbon solvent is one or more of nonane, decane and undecane;
the alcohol ether solvent is one or more of 3-butoxy-1-propanol, 1-butoxy-2-propanol, 2-tert-butoxyethanol and 3-methoxy-3-methyl-1-butanol;
the fine particle remover is one or more of HFC-4310mee, HFO-1336mzzZ, 3M7100 and 3M 7200;
the scaling powder remover is one or a mixture of 365AZ-M and 365 AZ-HM;
the whitening-resistant agent is diethylene glycol butyl ether;
the surface tension auxiliary agent is one or more of fatty alcohol polyoxyethylene ether, isomeric alcohol polyoxyethylene ether and alkylphenol polyoxyethylene ether.
2. The hydrocarbon cleaning agent for semiconductors as claimed in claim 1, wherein: the raw material also comprises 0.1-1.5 parts of fatty alcohol ether sodium sulfate and 0.2-2.4 parts of triethanolamine oleate.
3. A hydrocarbon cleaning agent for semiconductors as claimed in claim 1, wherein: the raw materials also comprise 1-3 parts of triethyl phosphate and 3-5 parts of diethyl ethylphosphonate.
4. A preparation method of the hydrocarbon cleaning agent for the semiconductor as claimed in claim 1, which comprises the following steps:
s1, weighing a hydrocarbon solvent, an alcohol ether solvent, a fine particle remover, a scaling powder remover, a whitening inhibitor and a surface tension auxiliary agent according to parts by weight;
s2, uniformly mixing a hydrocarbon solvent and an alcohol ether solvent to prepare a mixed solution A;
s3, uniformly mixing the fine particle remover, the soldering flux remover, the anti-whitening agent and the surface tension auxiliary agent to prepare a mixed solution B;
s4, pouring the mixed solution B into the mixed solution A, and uniformly stirring to obtain a mixed solution C;
s5, standing the mixed liquid C, and preparing a hydrocarbon cleaning agent finished product after the mixed liquid C is stable.
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