CN116042324A

CN116042324A - Oil removing powder for lead frame surface and preparation method thereof

Info

Publication number: CN116042324A
Application number: CN202310164506.5A
Authority: CN
Inventors: 邓麒俊; 吴家麟
Original assignee: Jiangmen Ubis Semiconductor Materials Co ltd
Current assignee: Jiangmen Ubis Semiconductor Materials Co ltd
Priority date: 2023-02-25
Filing date: 2023-02-25
Publication date: 2023-05-02

Abstract

The application relates to oil removal powder for the surface of a lead frame and a preparation method thereof, and relates to the technical field of oil stain products, wherein the oil removal powder comprises the following raw materials in parts by mass: 40-70 parts of sodium hydroxide, 15-25 parts of a magnetic phosphorus-free degreasing agent, 5-15 parts of sodium gluconate, 10-20 parts of sodium citrate, 1-5 parts of sodium dodecyl sulfate and 1-3 parts of a defoaming agent. The oil removing powder prepared by the method has a good oil removing effect, and meanwhile, the effect of polluting the environment can be effectively reduced.

Description

Oil removing powder for lead frame surface and preparation method thereof

Technical Field

The application relates to the technical field of oil stain products, in particular to oil removal powder for the surface of a lead frame and a preparation method thereof.

Background

The lead frame is a chip carrier of an integrated circuit, plays a role of a bridge connected with a new flat external wire, and oil removal liquid prepared by taking oil removal powder as a raw material can effectively remove oil stains on the surface of the lead frame; the degreasing powder is a low-foam degreasing agent refined by adopting a plurality of high-quality surfactants, detergents, penetrants, builders and the like. The method mainly uses the saponification reaction of alkali on ester substances in oil and the emulsification of a surfactant to remove greasy dirt on the metal surface.

Chinese patent application publication CN109183052A discloses an oil removing powder comprising 10-20 parts of sodium hydroxide, 5-10 parts of triethanolamine oleate soap, 30-40 parts of sodium carbonate, 5-10 parts of borax, 10-15 parts of coconut diethanol amine, 1-3 parts of sodium tripolyphosphate, 5-10 parts of a washing auxiliary agent, 10-15 parts of a metal protective agent and 1-2 parts of a surfactant. When in use, the oil removing powder has good wetting, solubilizing and emulsifying capabilities and strong oil removing capability.

In view of the above-mentioned related art, the inventor considers that when the oil removing powder directly discharges the waste water generated after the oil removing on the surface of the lead frame is completed, although sodium tripolyphosphate in the oil removing powder has good positive significance for improving the oil removing effect of the oil removing powder, the sodium tripolyphosphate contains phosphorus element, which is easy to cause eutrophication of water body and cause mass propagation of aquatic plants such as algae, and aerobic respiration of plant body consumes a large amount of oxygen in water to cause hypoxia death of aquatic animals, so that improvement is needed.

Disclosure of Invention

In order to enable the oil removing powder to have a good oil removing effect and reduce pollution to the environment, the application provides the oil removing powder for the surface of the lead frame and a preparation method of the oil removing powder.

In a first aspect, the application provides an oil removing powder for a surface of a lead frame, which adopts the following technical scheme: the oil removing powder for the surface of the lead frame comprises the following raw materials in parts by mass: 40-70 parts of sodium hydroxide, 15-25 parts of magnetic degreasing agent, 5-15 parts of sodium gluconate, 10-20 parts of sodium citrate, 1-5 parts of sodium dodecyl sulfate and 1-3 parts of defoaming agent.

By adopting the technical scheme, when the magnetic phosphorus-free oil removing agent is added into the oil removing powder, the magnetic oil removing agent can achieve better oil removing effect by being matched with sodium hydroxide, and the system does not contain phosphorus element, so that the pollution to the environment is reduced; sodium dodecyl sulfate can perform emulsification with oil globules, so that the oil globules are removed; sodium gluconate and sodium citrate are added into the oil removing powder, so that metal ions on the surface of the lead frame to be oil removed can be effectively complexed, the oil removing effect of sodium dodecyl sulfate on oil droplets is improved, and the oil removing performance of the oil removing powder is improved.

Because the sodium dodecyl sulfate is added into the oil removing powder, bubbles can be generated when the oil removing powder removes oil on the surface of the lead frame; the defoaming agent can reduce bubbles generated in the oil removal process, so that the oil removal effect of the oil removal powder is improved.

Preferably, the magnetic phosphorus-free degreasing agent is prepared by the following steps:

adding nano ferroferric oxide and chitosan into glycol solution to prepare a first mixture, sequentially drying and cooling the first mixture, separating out a solid mixture after cooling, and sequentially cleaning and drying the solid mixture to prepare the magnetic phosphorus-free degreasing agent.

Because some interfacial active substances such as naphthenic acid exist in the greasy dirt, the naphthenic acid is anionic, so the surface of the oil bead has negative charges, by adopting the technical scheme, the nano ferroferric oxide has positive charges, the specific surface area is large, the surface energy is high, the oil bead is easy to adsorb under the action of charges, and the surface of the oil bead is wrapped with a layer of magnetic particles, so the oil bead is removed.

The molecular chain of the chitosan contains rich amino groups, and the inventor discovers through a plurality of experiments that when the chitosan and the nano ferroferric oxide are mixed, the specific surface area of the nano ferroferric oxide is effectively increased, so that the removal effect of the nano ferroferric oxide on oil beads is improved.

Preferably, the mass ratio of the nano ferroferric oxide to the chitosan is 1 (0.3-0.5).

By adopting the technical scheme, the mass ratio of the nano ferroferric oxide to the chitosan is controlled within the range, so that the oil removal performance of the magnetic phosphorus-free oil remover is effectively improved.

Preferably, the nano ferroferric oxide is obtained after modification treatment, and the modification method of the nano ferroferric oxide is as follows:

adding nano ferroferric oxide into dilute hydrochloric acid to obtain a second mixture, controlling the pH value of the second mixture to be 9, adding oleic acid to react, separating solid after the reaction is finished, and sequentially cleaning and airing the solid to obtain the modified nano ferroferric oxide.

Because the nano ferroferric oxide is easy to generate agglomeration phenomenon in the system, the dispersibility of the nano ferroferric oxide is poor, and the use effect of the prepared magnetic phosphorus-free degreasing agent is easy to be influenced.

By adopting the technical scheme, oleic acid is a nonionic surfactant and has hydrophilic carboxyl groups and lipophilic alkyl chains; the carboxyl in oleic acid and the hydroxyl in nano ferroferric oxide form a stable hydrogen bond structure, so that an alkyl chain tends to the outer side, and an oil-philic film is formed on the surface of nano ferroferric oxide particles, thereby forming a steric hindrance effect; due to the existence of the steric hindrance effect, van der Waals force and chemical bonds among nano ferroferric oxide particles can be inhibited, so that agglomeration among the nano ferroferric oxide particles is reduced, and the dispersibility of the nano ferroferric oxide is further improved.

Preferably, the mass ratio of the nano ferroferric oxide to the oleic acid is 1 (0.05-0.09).

By adopting the technical scheme, the mass ratio of the nano ferroferric oxide to the oleic acid is controlled within the range, so that the dispersion performance of the nano ferroferric oxide is effectively improved.

Preferably, the defoamer is a silicone defoamer.

In a second aspect, the present application provides a method for preparing oil-removing powder for a surface of a lead frame, which adopts the following technical scheme:

mixing sodium hydroxide, magnetic phosphorus-free degreasing agent, sodium gluconate, sodium citrate, sodium dodecyl sulfate and defoaming agent, and stirring uniformly to obtain the degreasing powder.

In a third aspect, the present application provides a working solution, where the working solution is prepared from oil removal powder as a raw material, and the specific preparation steps are as follows:

adding the oil removing powder into the heated deionized water, stirring until the oil removing powder is dissolved, and then adding the deionized water to dilute the oil removing powder to a required liquid level to prepare the working solution.

Preferably, the working fluid can be used for hot dip degreasing, ultrasonic degreasing and electrolytic degreasing.

In summary, the present application includes at least one of the following beneficial technical effects:

1. when the magnetic phosphorus-free oil removing agent is added into the oil removing powder, the magnetic oil removing agent can achieve better oil removing effect by being matched with sodium hydroxide, and the system does not contain phosphorus element, so that the pollution to the environment is reduced.

2. The nano ferroferric oxide has positive charges, and the oil beads can be adsorbed through the action of the charges, so that the surfaces of the oil beads are wrapped with a layer of magnetic particles, and the oil beads are removed. The molecular chain of the chitosan contains rich amino groups, and the inventor discovers through a plurality of experiments that when the chitosan and the nano ferroferric oxide are mixed, the specific surface area of the nano ferroferric oxide is effectively increased, so that the removal effect of the nano ferroferric oxide on oil droplets is improved.

3. Oleic acid is a nonionic surfactant, and can form a layer of oil-philic film on the surfaces of nano ferroferric oxide particles, so that a steric hindrance effect is formed, van der Waals force and chemical bonds between the nano ferroferric oxide particles are inhibited due to the existence of the steric hindrance effect, and the dispersibility of the nano ferroferric oxide is further improved.

Detailed Description

The embodiment of the application discloses oil removing powder for the surface of a lead frame and a preparation method thereof.

Example 1

An oil removing powder for the surface of a lead frame comprises the following raw materials in parts by weight: 40g of sodium hydroxide, 15g of magnetic phosphorus-free degreasing agent, 5g of sodium gluconate, 10g of sodium citrate, 1g of sodium dodecyl sulfate and 1g of defoaming agent.

The oil removing powder is prepared by the following steps:

Wherein the magnetic phosphorus-free degreasing agent comprises the following raw materials by weight: 10g of nano ferroferric oxide and 3g of chitosan.

The magnetic phosphorus-free degreasing agent is prepared by the following steps:

adding nano ferroferric oxide and chitosan into 60g of ethylene glycol solution (the mass concentration of the ethylene glycol solution is 80%) to prepare a first mixture, putting the first mixture into a 185 ℃ oven for drying for 48 hours, cooling to 27 ℃, separating a solid mixture by using a magnet, washing the solid mixture with ethanol and ultrapure water for three times, and finally putting the solid mixture into a 60 ℃ vacuum drying box for drying for 12 hours to prepare the magnetic phosphorus-free degreasing agent.

Wherein the defoaming agent is an organosilicon defoaming agent.

Example 2

An oil removing powder for the surface of a lead frame comprises the following raw materials in parts by weight: 70g of sodium hydroxide, 25g of magnetic phosphorus-free degreasing agent, 15g of sodium gluconate, 20g of sodium citrate, 5g of sodium dodecyl sulfate and 3g of defoaming agent.

The oil removing powder is prepared by the following steps:

Wherein the magnetic phosphorus-free degreasing agent comprises the following raw materials by weight: 10g of nano ferroferric oxide and 5g of chitosan.

Wherein the defoaming agent is an organosilicon defoaming agent.

Example 3

An oil removing powder for the surface of a lead frame comprises the following raw materials in parts by weight: 55g of sodium hydroxide, 20g of magnetic phosphorus-free degreasing agent, 10g of sodium gluconate, 15g of sodium citrate, 3g of sodium dodecyl sulfate and 2g of defoaming agent.

The oil removing powder is prepared by the following steps:

Wherein the magnetic phosphorus-free degreasing agent comprises the following raw materials by weight: 10g of nano ferroferric oxide and 4g of chitosan.

Wherein the defoaming agent is an organosilicon defoaming agent.

Example 4

Example 4 differs from example 3 in that: 12.7g of nano ferroferric oxide and 1.3g of chitosan.

Example 5

Example 5 differs from example 3 in that: 8.2g of nano ferroferric oxide and 5.8g of chitosan.

Example 6

Example 6 differs from example 3 in that: the nano ferroferric oxide is obtained after modification treatment, and the modification method of the nano ferroferric oxide is as follows:

10g of nano ferroferric oxide is added into dilute hydrochloric acid to obtain a second mixture, the pH of the second mixture is controlled to be 9, 0.5g of oleic acid is added to react for 20min, the solid is separated, and the solid is firstly washed 3 times with distilled water and then 3 times with anhydrous methanol, and then dried to obtain the modified nano ferroferric oxide.

Example 7

Example 7 differs from example 3 in that: the nano ferroferric oxide is obtained after modification treatment, and the modification method of the nano ferroferric oxide is as follows:

10g of nano ferroferric oxide is added into dilute hydrochloric acid to obtain a second mixture, the pH of the second mixture is controlled to be 9, 0.9g of oleic acid is added to react for 20min, the solid is separated, and the solid is firstly washed 3 times with distilled water and then 3 times with anhydrous methanol, and then dried to obtain the modified nano ferroferric oxide.

Example 8

Example 8 differs from example 3 in that: the nano ferroferric oxide is obtained after modification treatment, and the modification method of the nano ferroferric oxide is as follows:

10g of nano ferroferric oxide is added into dilute hydrochloric acid to obtain a second mixture, the pH of the second mixture is controlled to be 9, 0.7g of oleic acid is added to react for 20min, the solid is separated, and the solid is firstly washed 3 times with distilled water and then 3 times with anhydrous methanol, and then dried to obtain the modified nano ferroferric oxide.

Example 9

Example 9 differs from example 8 in that: the nano ferroferric oxide is obtained after modification treatment, and the modification method of the nano ferroferric oxide is as follows:

10.5g of nano ferroferric oxide is added into dilute hydrochloric acid to obtain a second mixture, the pH value of the second mixture is controlled to be 9, 0.2g of oleic acid is added for reaction for 20min, the solid is separated, and the solid is firstly washed 3 times with distilled water and then 3 times with absolute methanol, and then dried to obtain the modified nano ferroferric oxide.

Example 10

Example 10 differs from example 8 in that: the nano ferroferric oxide is obtained after modification treatment, and the modification method of the nano ferroferric oxide is as follows:

adding 9.6g of nano ferroferric oxide into dilute hydrochloric acid to obtain a second mixture, controlling the pH of the second mixture to be 9, adding 1.1g of oleic acid, reacting for 20min, separating solid, washing with distilled water for 3 times, washing with absolute methanol for 3 times, and airing to obtain the modified nano ferroferric oxide.

Example 11

Example 11 differs from example 3 in that: 14g of nano ferroferric oxide and 0g of chitosan.

Comparative example 1

Comparative example 1 and example 3 differ in that: no antifoaming agent is added into the oil removal powder.

Application examples 1-12 are hot dip degreasing working fluids.

Application example 1

The working solution comprises the following raw materials by weight: 100g of the oil removal powder prepared in example 1 and 1L of deionized water.

The working solution is prepared by the following steps:

firstly, mixing oil removing powder with 400mL of deionized water heated to 30 ℃, then adding the oil removing powder, stirring until the oil removing powder is dissolved, and then adding 600mL of deionized water to prepare the working solution.

The application examples 2 to 12 are different from the application example 1 in that the oil removing powder is prepared in different examples, and the correspondence between the oil removing powder prepared in specific examples and the application example is shown in the following table 1.

TABLE 1

Application example 2	Example 2
		Application example 3	Example 3
Application example 4	Example 4
		Application example 5	Example 5
Application example 6	Example 6
		Application example 7	Example 7
Application example 8	Example 8
		Application example 9	Example 9
Application example 10	Example 10
		Application example 11	Example 11
Application example 12	Comparative example 1

Application examples 13-24 are ultrasonic oil removing working fluids.

Application example 13

The working solution comprises the following raw materials by weight: 75g of oil removal powder prepared in example 1 and 1L of deionized water.

The working solution is prepared by the following steps:

firstly, mixing oil removing powder with 400mL of deionized water heated to 60 ℃, then adding the oil removing powder, stirring until the oil removing powder is dissolved, and then adding 600mL of deionized water to prepare the working solution.

Application examples 14 to 24 are different from application example 13 in that the oil removing powder is prepared in different examples, and the correspondence between the oil removing powder prepared in specific examples and application examples is shown in the following table 2.

TABLE 2

Application example 14	Example 2
		Application example 15	Example 3
Application example 16	Example 4
		Application example 17	Example 5
Application example 18	Example 6
		Application example 19	Example 7
Application example 20	Example 8
		Application example 21	Example 9
Application example 22	Example 10
		Application example 23	Example 11
Application example 24	Comparative example 1

Application examples 25-36 are electrolytic degreasing working fluids.

Application example 25

The working solution is prepared by the following steps:

firstly, mixing oil removing powder, 10g of sodium hydroxide and 400mL of deionized water heated to 60 ℃, then adding the oil removing powder, stirring until the oil removing powder is dissolved, and then adding 600mL of deionized water to prepare the working solution.

Application examples 26 to 36 are different from application example 25 in that the oil-removing powder is prepared in different examples, and the correspondence between the oil-removing powder prepared in specific examples and application examples is shown in the following table 3.

TABLE 3 Table 3

And (3) oil removal performance detection: (Artificial oil stain reference standard JB/T4323) with strip steel as detection sample

Hot dipping; cleaning the surface of the strip steel sequentially by isopropanol, ethanol and distilled water, drying and weighing to obtain m1, uniformly coating artificial oil stains on the surface of the strip steel, standing for 20min, scraping oil stains gathered at the lower end, weighing to obtain m2, immersing the strip steel after scraping the oil stains gathered at the lower end in the working solution prepared in application examples 1-12 heated to 80 ℃ for 1min, drying, and weighing to obtain m3.

Ultrasonic method: cleaning the surface of the strip steel sequentially by isopropanol, ethanol and distilled water, drying and weighing to obtain m1, uniformly coating artificial oil stains on the surface of the strip steel, standing for 20min, scraping oil stains gathered at the lower end, weighing to obtain m2, immersing the strip steel after scraping the oil stains gathered at the lower end in an application example 13-24 heated to 60 ℃ for 0.5min in a working solution under an ultrasonic environment with ultrasonic frequency of 30KHz, drying, and weighing to obtain m3.

Electrolytic method: cleaning the surface of the strip steel sequentially by isopropanol, ethanol and distilled water, drying, weighing and marking as m1, uniformly coating artificial oil stains on the surface of the strip steel, standing for 20min, scraping oil stains gathered at the lower end, weighing and marking as m2, immersing the strip steel with current density of 2-20ASD under the electrolysis condition, scraping the oil stains gathered at the lower end in an application example 25-36 heated to 60 ℃ to prepare working solution for 0.5min, drying, and weighing and marking as m3.

The oil removal rate was calculated by the hot dipping method, ultrasonic method and electrolytic method according to the following formulas

Wherein: m1: the weight (g) of the unoiled strip;

m2: the weight (g) of the strip steel after oiling;

m3: and (g) the weight of the strip steel after oil removal and drying.

TABLE 4 Table 4

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Data analysis

As can be seen from Table 4, the oil removal rate of the hot dip method in examples 1-3 is 85.7-86.3%, the oil removal rate of the ultrasonic method is 90.8-91.4%, and the oil removal rate of the electrolytic method is 95.2-95.9%, so that it can be seen that the oil removal powder prepared by the present application has good oil removal performance.

From table 4, it can be seen that the difference between example 4 and example 3 is: in example 3, 10g of nano ferroferric oxide, 4g of chitosan, 12.7g of nano ferroferric oxide, 1.3g of chitosan, and the oil removing effect is obviously reduced compared with example 3, because when the content of chitosan is reduced, the specific surface area of nano ferroferric oxide is reduced, so that the adsorption effect of nano ferroferric oxide on oil beads through the charge effect is weakened, and the oil removing performance of oil removing powder is reduced.

From table 4, it can be seen that the difference between example 5 and example 3 is: in example 3, 10g of nano ferroferric oxide, 4g of chitosan, 8.2g of nano ferroferric oxide in example 5, 5.8g of chitosan, and the oil removing effect is obviously reduced compared with example 3, because when the content of nano ferroferric oxide is reduced, the adsorption effect of nano ferroferric oxide on oil droplets is reduced by the charge effect, so that the oil removing performance of oil removing powder is reduced.

As can be seen from Table 4, examples 6-8 differ from example 3 in that: the nano ferroferric oxide in the examples 6-8 is obtained after modified treatment, the nano ferroferric oxide in the example 3 is not modified, and the oil removing effect is obviously improved compared with that in the example 3 because the surface of the nano ferroferric oxide is formed with an oil-philic film to form a steric hindrance effect, so that the agglomeration phenomenon among the nano ferroferric oxide is reduced, the adsorption effect of the nano ferroferric oxide on oil droplets through the charge effect is enhanced, and the oil removing performance of oil removing powder is further improved.

From Table 4, it can be seen that the difference between example 9 and example 8 is: in the embodiment 8, 10g of nano ferroferric oxide, 0.7g of oleic acid, 10.5g of nano ferroferric oxide in the embodiment 9 and 0.2g of oleic acid, compared with the embodiment 9 and the embodiment 8, the oil removing effect is obviously reduced, because when the content of oleic acid is reduced, a part of nano ferroferric oxide still has no oil-philic film formed on the surface, so that the agglomeration phenomenon of part of nano ferroferric oxide is caused, the adsorption effect of nano ferroferric oxide on oil beads is weakened through the charge effect, and the oil removing performance of oil removing powder is further reduced.

As can be seen from table 4, the difference between example 10 and example 8 is that: in the embodiment 8, 10g of nano ferroferric oxide, 0.7g of oleic acid, 9.6g of nano ferroferric oxide in the embodiment 10 and 1.1g of oleic acid are obviously reduced compared with the embodiment 10 and the embodiment 8, because when the content of oleic acid is increased, oleic acid is repeatedly coated, and excessive oleic acid can cause the modified nano ferroferric oxide to be adsorbed and mutually adhered and wound, the particle size of the nano ferroferric oxide is increased, so that the adsorption effect of the nano ferroferric oxide on oil droplets is reduced by the charge effect, and the oil removing performance of oil removing powder is reduced.

As can be seen from table 4, the difference between example 11 and example 3 is that: in example 3, 10g of nano ferroferric oxide, 4g of chitosan, 14g of nano ferroferric oxide and 0g of chitosan in example 11, the oil removing effect is obviously reduced compared with example 3, because when the magnetic phosphorus-free oil removing agent does not contain chitosan, the adsorption effect of the magnetic phosphorus-free oil removing agent on oil droplets is weakened, and the oil removing performance of the oil removing powder is reduced.

From table 4, the difference between comparative example 1 and example 3 is: in example 3, the antifoaming agent was contained, and in comparative example 1, the antifoaming agent was not contained, and the degreasing effect was remarkably reduced as compared with example 3, because the antifoaming agent was not contained in the degreasing powder, and thus bubbles were generated during degreasing, and the degreasing performance of the degreasing powder was reduced.

The present embodiment is merely illustrative of the present application, and the present application is not limited thereto, and a worker can make various changes and modifications without departing from the scope of the technical idea of the present application. The technical scope of the present application is not limited to the contents of the specification, and must be determined according to the scope of claims.

Claims

1. An oil removing powder for a surface of a lead frame, characterized in that: the material comprises the following raw materials in parts by mass: 40-70 parts of sodium hydroxide, 15-25 parts of a magnetic phosphorus-free degreasing agent, 5-15 parts of sodium gluconate, 10-20 parts of sodium citrate, 1-5 parts of sodium dodecyl sulfate and 1-3 parts of a defoaming agent.

2. A degreasing powder for a surface of a lead frame according to claim 1, wherein: the magnetic phosphorus-free degreasing agent is prepared by the following steps:

3. A degreasing powder for a surface of a lead frame according to claim 2, wherein: the mass ratio of the nano ferroferric oxide to the chitosan is 1 (0.3-0.5).

4. The degreasing powder for a lead frame surface according to claim 2, wherein: the nano ferroferric oxide is obtained after modification treatment, and the modification method of the nano ferroferric oxide comprises the following steps:

5. The degreasing powder for a surface of a lead frame according to claim 4, wherein: the mass ratio of the nano ferroferric oxide to the oleic acid is 1 (0.05-0.09).

6. A degreasing powder for a surface of a lead frame according to claim 1, wherein: the defoaming agent is an organosilicon defoaming agent.

7. A method for preparing the degreasing powder for lead frame surfaces as claimed in claims 1 to 6, characterized in that: the method comprises the following steps:

8. The working solution is prepared from the oil removal powder prepared by the method of claim 7 as a raw material, and comprises the following specific preparation steps:

9. A working fluid as set forth in claim 8 wherein: the working solution can be used for hot dip degreasing, ultrasonic degreasing and electrolytic degreasing.