CN109810806B - Flame-retardant electronic cleaning agent and preparation method thereof - Google Patents
Flame-retardant electronic cleaning agent and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the field of fine chemical engineering, in particular to a flame-retardant electronic cleaning agent and a preparation method thereof; the invention discloses a flame-retardant electronic cleaning agent and a preparation method thereof. And a fluorine-containing cosolvent is added, so that the cleaning ability of the cleaning agent can be further improved; the cleaning agent has the characteristics of flame retardance, no flash point and an ODP (ozone depletion potential) value of 0, and has good compatibility with most plastic materials.
Description
Technical Field
The invention relates to the field of fine chemical engineering, in particular to a flame-retardant electronic cleaning agent and a preparation method thereof.
Background
With the rapid development of electronic products toward miniaturization, high density and high reliability, more and more pollutants are introduced in the process of electronic manufacturing process, and if the pollutants cannot be removed in time, the smooth implementation of the process or the quality and reliability of the product are inevitably affected. Therefore, in order to ensure the smooth progress of the electronic manufacturing process and the quality and reliability of the manufactured products, it is necessary to introduce a cleaning process and use a cleaning agent in many steps of the process implementation.
CN104152298A discloses a precision electronic cleaning agent, which comprises the following raw materials, by mass, 75-80 parts of a halogen-containing compound, 8-15 parts of an organic solvent and 5-10 parts of a monohydric alcohol. The halogen-containing compound which has extremely small damage to the ozone layer is used as a main cleaning agent, and a proper organic solvent and monohydric alcohol are used as auxiliary agents for cleaning precise electrons, so that the effects of high cleaning activity and reduction of environmental pollution are achieved.
CN105349270A provides a nonaqueous electronic cleaning agent and a preparation method thereof. The electronic cleaning agent comprises the following components: citrus oil, acetyl tributyl citrate, calcium stearoyl lactate, potassium silicate, sodium alginate, sorbitol, dibasic lead stearate, sodium carbonate, sodium citrate, TBHQ, sodium dehydroacetate, ethanol and water. The preparation method comprises the steps of mixing TBHQ, acetyl tributyl citrate and ethanol to obtain a solution A, mixing citrus oil, calcium stearoyl lactylate, potassium silicate, sodium alginate, sorbitol, dibasic lead stearate, sodium carbonate, sodium citrate, sodium dehydroacetate and water, heating and stirring to obtain a solution B; and adding the solution A after the solution is cooled, and uniformly stirring to obtain the product. The cleaning agent has high cleaning efficiency, does not corrode electronic equipment, does not harm human bodies, is easy to degrade and does not pollute the environment; and the preparation method is simple, easy to control, easy for industrial production and low in production cost.
CN103194331A provides an electronic cleaning agent and a preparation method thereof, which comprises the following components in percentage by weight: 10-40% of low molecular alcohols, 30-50% of methyl siloxane and 30-40% of low molecular ketones. The cleaning agent can improve the cleaning efficiency of the lead-free welding residues, meets the environment-friendly requirement, and can safely pass various inspection applications.
The electronic cleaning agent prepared by the above patents and the prior art does not have a flame retardant effect, and the application of the electronic cleaning agent is increasingly limited today with the ever-increasing fire prevention and safety awareness.
Disclosure of Invention
In order to solve the problems, the invention provides a flame-retardant electronic cleaning agent and a preparation method thereof.
The flame-retardant electronic cleaning agent and the preparation method thereof are carried out according to the following scheme:
adding 18.67-32.74 parts of dichloroethylene and 0.1-0.5 part of fluorine-containing cosolvent into a reaction kettle according to the mass parts, controlling the temperature to be 35-45 ℃, stirring for 10-20min, then adding 24.78-41.25 parts of perfluorohexanone into the reaction kettle, and continuing to keep the temperature and stir for 1-5 h; and after stirring, adding 0.01-0.8 part of 4,4 ', 4 ' ' -tris (4, 5-dichlorophthalimidophenyl) methyl bromide, 5.67-10.41 parts of hexafluoropropyl methyl ether, 0.05-0.15 part of bismuth succinate, 0.08-0.2 part of 5, 6-diamino-2, 3-dicyanopyrazine and 0.04-0.2 part of 6- (4-morpholinyl) -3-pyridine boric acid, heating to the final reaction temperature, stirring for 10-15h, and cooling to room temperature after stirring to obtain the flame retardant electronic cleaning agent.
The reaction kettle is a sealed pressure-resistant reaction kettle and can bear the pressure of not more than 3 MPa.
The dichloroethylene is trans-dichloroethylene.
The final reaction temperature is 40-50 ℃.
The fluorine-containing cosolvent is prepared according to the following scheme:
adding 25.6-38.5 parts of dodecafluorooctanedioic acid and 80-150 parts of toluene into a reaction kettle, controlling the temperature at 60-70 ℃, stirring and mixing for 10-15min, then adding 14.3-19.7 parts of diethanolamine into the flask, uniformly stirring, heating to 150 ℃ for stirring reaction, stirring for 300min, after the reaction is finished, distilling the solvent under reduced pressure, then adding 2.8-5.6 parts of isopropyl 2-iodoacyl-benzoate and 0.5-3.5 parts of triglycerol monostearate into the reaction kettle, controlling the temperature at 70-80 ℃, stirring for 250min for 130min, and cooling to room temperature after the reaction is finished, thus obtaining the fluorine-containing cosolvent.
The invention discloses a flame-retardant electronic cleaning agent and a preparation method thereof. The cleaning agent has the characteristics of flame retardance, no flash point and an ODP (ozone depletion potential) value of 0, and has good compatibility with most plastic materials.
Drawings
FIG. 1 is an infrared spectrum of a sample of a flame retardant electronic cleaning agent prepared according to the process of example 1.
Detailed Description
The invention is further illustrated by the following specific examples:
example 1
The flame-retardant electronic cleaning agent and the preparation method thereof are carried out according to the following scheme:
adding 25.61 parts of dichloroethylene and 0.3 part of fluorine-containing cosolvent into a reaction kettle according to the mass parts, controlling the temperature to be 40 ℃, stirring for 15min, then adding 28.51 parts of perfluorohexanone into the reaction kettle, and continuing to keep the temperature and stir for 3 h; and after stirring, adding 0.06 part of 4,4 ', 4 ' ' -tris (4, 5-dichlorophthalimidophenyl) methyl bromide, 8.24 parts of hexafluoropropyl methyl ether, 0.1 part of bismuth succinate, 0.14 part of 5, 6-diamino-2, 3-dicyanopyrazine and 0.12 part of 6- (4-morpholinyl) -3-pyridineboronic acid, heating to a final reaction temperature, stirring for 13 hours, and cooling to room temperature after stirring is finished to obtain the flame retardant type electronic cleaning agent.
The reaction kettle is a sealed pressure-resistant reaction kettle and can bear the pressure of not more than 3 MPa.
The dichloroethylene is trans-dichloroethylene.
The final reaction temperature was 45 ℃.
The fluorine-containing cosolvent is prepared according to the following scheme:
adding 31.4 parts by weight of dodecafluorosuberic acid and 120 parts by weight of toluene into a reaction kettle, controlling the temperature at 65 ℃, stirring and mixing for 13min, adding 17.2 parts of diethanolamine into a flask, uniformly stirring, heating to 130 ℃, stirring and reacting for 240min, after the reaction is finished, distilling off the solvent under reduced pressure, adding 4.2 parts of 2-iodoacyl-benzoic acid isopropyl ester and 2.5 parts of triglycerol monostearate into the reaction kettle, controlling the temperature at 75 ℃, stirring for 190min, and cooling to room temperature after the reaction is finished, thus obtaining the fluorine-containing cosolvent.
Example 2
The flame-retardant electronic cleaning agent and the preparation method thereof are carried out according to the following scheme:
adding 18.67 parts of dichloroethylene and 0.1 part of fluorine-containing cosolvent into a reaction kettle according to the mass parts, controlling the temperature to be 35 ℃, stirring for 10min, then adding 24.78 parts of perfluorohexanone into the reaction kettle, and continuing to stir for 1h under heat preservation; and after stirring, adding 0.01 part of 4,4 ', 4 ' ' -tris (4, 5-dichlorophthalimidophenyl) methyl bromide, 5.67 parts of hexafluoropropyl methyl ether, 0.05 part of bismuth succinate, 0.08 part of 5, 6-diamino-2, 3-dicyanopyrazine and 0.04 part of 6- (4-morpholinyl) -3-pyridineboronic acid, heating to a final reaction temperature, stirring for 10 hours, and cooling to room temperature after stirring to obtain the flame retardant type electronic cleaning agent.
The reaction kettle is a sealed pressure-resistant reaction kettle and can bear the pressure of not more than 3 MPa.
The dichloroethylene is trans-dichloroethylene.
The final reaction temperature was 40 ℃.
The fluorine-containing cosolvent is prepared according to the following scheme:
adding 25.6 parts by weight of dodecafluorosuberic acid and 80 parts by weight of toluene into a reaction kettle, controlling the temperature at 60 ℃, stirring and mixing for 10min, adding 14.3 parts of diethanolamine into a flask, uniformly stirring, heating to 120 ℃, stirring and reacting for 200min, after the reaction is finished, distilling off the solvent under reduced pressure, adding 2.8 parts of 2-iodoacyl-benzoic acid isopropyl ester and 0.5 part of triglycerol monostearate into the reaction kettle, controlling the temperature at 70 ℃, stirring for 130min, and cooling to room temperature after the reaction is finished, thus obtaining the fluorine-containing cosolvent.
Example 3
The flame-retardant electronic cleaning agent and the preparation method thereof are carried out according to the following scheme:
adding 32.74 parts of dichloroethylene and 0.5 part of fluorine-containing cosolvent into a reaction kettle according to the mass parts, controlling the temperature to be 45 ℃, stirring for 20min, then adding 41.25 parts of perfluorohexanone into the reaction kettle, and continuing to keep the temperature and stir for 5 h; and after stirring, adding 0.8 part of 4,4 ', 4 ' ' -tris (4, 5-dichlorophthalimidophenyl) methyl bromide, 10.41 parts of hexafluoropropyl methyl ether, 0.15 part of bismuth succinate, 0.2 part of 5, 6-diamino-2, 3-dicyanopyrazine and 0.2 part of 6- (4-morpholinyl) -3-pyridineboronic acid, heating to a final reaction temperature, stirring for 15 hours, and cooling to room temperature after stirring to obtain the flame retardant type electronic cleaning agent.
The reaction kettle is a sealed pressure-resistant reaction kettle and can bear the pressure of not more than 3 MPa.
The dichloroethylene is trans-dichloroethylene.
The final reaction temperature was 50 ℃.
The fluorine-containing cosolvent is prepared according to the following scheme:
adding 38.5 parts by weight of dodecafluorooctanedioic acid and 150 parts by weight of toluene into a reaction kettle, controlling the temperature at 70 ℃, stirring and mixing for 15min, adding 19.7 parts of diethanolamine into a flask, uniformly stirring, heating to 150 ℃, stirring and reacting for 300min, after the reaction is finished, distilling off the solvent under reduced pressure, adding 5.6 parts of isopropyl 2-iodoacyl-benzoate and 3.5 parts of triglycerol monostearate into the reaction kettle, controlling the temperature at 80 ℃, stirring for 250min, and cooling to room temperature after the reaction is finished, thus obtaining the fluorine-containing cosolvent.
Example 4
The flame-retardant electronic cleaning agent and the preparation method thereof are carried out according to the following scheme:
adding 32.74 parts of dichloroethylene and 0.5 part of fluorine-containing cosolvent into a reaction kettle according to the mass parts, controlling the temperature to be 45 ℃, stirring for 20min, then adding 41.25 parts of perfluorohexanone into the reaction kettle, and continuing to keep the temperature and stir for 5 h; and after stirring, adding 0.3 part of 4,4 ', 4 ' ' -tris (4, 5-dichlorophthalimidophenyl) methyl bromide, 10.41 parts of hexafluoropropyl methyl ether, 0.08 part of bismuth succinate, 0.14 part of 5, 6-diamino-2, 3-dicyanopyrazine and 0.15 part of 6- (4-morpholinyl) -3-pyridineboronic acid, heating to a final reaction temperature, stirring for 12 hours, and cooling to room temperature after stirring to obtain the flame retardant type electronic cleaning agent.
The reaction kettle is a sealed pressure-resistant reaction kettle and can bear the pressure of not more than 3 MPa.
The dichloroethylene is trans-dichloroethylene.
The final reaction temperature was 45 ℃.
The fluorine-containing cosolvent is prepared according to the following scheme:
adding 25.6 parts by weight of dodecafluorosuberic acid and 80 parts by weight of toluene into a reaction kettle, controlling the temperature at 60 ℃, stirring and mixing for 10min, adding 14.3 parts of diethanolamine into a flask, uniformly stirring, heating to 120 ℃, stirring and reacting for 200min, after the reaction is finished, distilling off the solvent under reduced pressure, adding 2.8 parts of 2-iodoacyl-benzoic acid isopropyl ester and 0.5 part of triglycerol monostearate into the reaction kettle, controlling the temperature at 70 ℃, stirring for 130min, and cooling to room temperature after the reaction is finished, thus obtaining the fluorine-containing cosolvent.
Comparative example 1
This comparative example was conducted under the conditions of example 1, except that no fluorine-containing co-solvent was added.
Comparative example 2
This comparative example was conducted under the conditions of example 1 except that no perfluorohexanone was added.
Comparative example 3
This comparative example was conducted under the conditions of example 1 except that 4,4 ', 4 ' ' -tris (4, 5-dichlorophthalimidophenyl) methyl bromide was not added.
Comparative example 4
This comparative example was conducted under the conditions of example 1, except that bismuth succinate was not added.
Comparative example 5
This comparative example was conducted under the conditions of example 1 except that 5, 6-diamino-2, 3-dicyanopyrazine was not added.
Comparative example 6
This comparative example was conducted under the conditions of example 1 except that 6- (4-morpholinyl) -3-pyridineboronic acid was not added.
Comparative example 7
This comparative example was conducted under the conditions of example 1 except that hexafluoropropyl methyl ether was not added.
And (4) performing infrared spectrum analysis on the synthesized product by using a Fourier transform infrared spectrometer and a potassium bromide single chip. From the infrared spectrum of the product synthesized in example 1, it is known that: the product is at 1000-1400cm-1Has a strong band in the range, which is mainly caused by stretching vibration of C-F bond, at 1660cm-1A characteristic absorption peak of C = O bond is nearby, 2850-3000cm-1The band in the range is C-H bond stretching vibration of methyl; the product is at 650cm-1A characteristic absorption peak of Bi-OH bonds is nearby; 640-648cm-1Nearby has C-Br elongationA contraction vibration absorption peak; the product is in 2264cm-1A characteristic absorption peak of a cyano group (C.ident.N) in the vicinity thereof; the product was at 1420cm-1The characteristic absorption peak of B-OH bond is nearby.
According to the IPC-TM-6502.3.25 standard, a ZI-100A cleanliness tester is adopted to test the cleaning ability of the cleaning agent; the flame retardant property of the cleaning agent is measured according to GB/T2406-93.
The product quality indicators in the above examples are shown in the following table:
| item | Limiting oxygen index (OI%) | Detergency (μ g/cm)2） |
| Example 1 | 28.1 | 7.24 |
| Example 2 | 27.9 | 6.18 |
| Example 3 | 31.5 | 7.51 |
| Example 4 | 30.2 | 8.59 |
| Comparative example 1 | 26.7 | 4.64 |
| Comparative example 2 | 24.8 | 4.15 |
| Comparative example 3 | 26.6 | 4.97 |
| Comparative example 4 | 26.9 | 4.99 |
| Comparative example 5 | 27.1 | 5.12 |
| Comparative example 6 | 27.2 | 5.20 |
| Comparative example 7 | 24.7 | 3.90 |
Various modifications and alterations of this invention may be made by those skilled in the art without departing from the spirit and scope of this invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (4)
1. The preparation method of the flame-retardant electronic cleaning agent is carried out according to the following scheme:
adding 18.67-32.74 parts of dichloroethylene and 0.1-0.5 part of fluorine-containing cosolvent into a reaction kettle according to the mass parts, controlling the temperature to be 35-45 ℃, stirring for 10-20min, then adding 24.78-41.25 parts of perfluorohexanone into the reaction kettle, and continuing to keep the temperature and stir for 1-5 h; after stirring, adding 0.01-0.8 part of 4,4 ', 4 ' ' -tris (4, 5-dichlorophthalimidophenyl) methyl bromide, 5.67-10.41 parts of hexafluoropropyl methyl ether, 0.05-0.15 part of bismuth succinate, 0.08-0.2 part of 5, 6-diamino-2, 3-dicyanopyrazine and 0.04-0.1 part of 6- (4-morpholinyl) -3-pyridine boric acid, heating to the final reaction temperature, stirring for 10-15h, and cooling to room temperature after stirring to obtain the flame-retardant electronic cleaning agent;
the fluorine-containing cosolvent is prepared according to the following scheme:
adding 25.6-38.5 parts of dodecafluorooctanedioic acid and 80-150 parts of toluene into a reaction kettle, controlling the temperature at 60-70 ℃, stirring and mixing for 10-15min, then adding 14.3-19.7 parts of diethanolamine into the flask, uniformly stirring, heating to 150 ℃ for stirring reaction, stirring for 300min, after the reaction is finished, distilling the solvent under reduced pressure, then adding 2.8-5.6 parts of isopropyl 2-iodoacyl-benzoate and 0.5-3.5 parts of triglycerol monostearate into the reaction kettle, controlling the temperature at 70-80 ℃, stirring for 250min for 130min, and cooling to room temperature after the reaction is finished, thus obtaining the fluorine-containing cosolvent.
2. The preparation method of the flame-retardant electronic cleaning agent according to claim 1, characterized by comprising the following steps: the reaction kettle is a sealed pressure-resistant reaction kettle and can bear the pressure of not more than 3 MPa.
3. The preparation method of the flame-retardant electronic cleaning agent according to claim 1, characterized by comprising the following steps: the dichloroethylene is trans-dichloroethylene.
4. The preparation method of the flame-retardant electronic cleaning agent according to claim 1, characterized by comprising the following steps: the final reaction temperature is 40-50 ℃.
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| CN107481870A (en) * | 2017-09-08 | 2017-12-15 | 西安科技大学 | A kind of electrolytic solution for super capacitor and its ultracapacitor of preparation |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10399960B2 (en) * | 2015-11-10 | 2019-09-03 | Kyushu University, National University Corporation | Dicyanopyrazine compound, luminescent material, luminescence device using the same, and method for producing 2,5-dicyano-3,6-dihalogenopyrazine |
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| CN1727462A (en) * | 2001-11-02 | 2006-02-01 | 广州南沙经济技术开发区高奇环保技术有限公司 | Cleaning agent for electrified accurate electronic apparatus |
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| CN103265752A (en) * | 2013-06-04 | 2013-08-28 | 广东聚石化学股份有限公司 | Halogen-free flame retardant thermoplastic polyolefin cable material |
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| CN107481870A (en) * | 2017-09-08 | 2017-12-15 | 西安科技大学 | A kind of electrolytic solution for super capacitor and its ultracapacitor of preparation |
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