CN111910231B - Roughening liquid for roughening glass fiber reinforced plastic and roughening method - Google Patents
Roughening liquid for roughening glass fiber reinforced plastic and roughening method Download PDFInfo
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- CN111910231B CN111910231B CN202010711294.4A CN202010711294A CN111910231B CN 111910231 B CN111910231 B CN 111910231B CN 202010711294 A CN202010711294 A CN 202010711294A CN 111910231 B CN111910231 B CN 111910231B
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- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
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Abstract
The invention discloses roughening liquid and a roughening method for roughening glass fiber reinforced plastic, wherein hydrogen fluoride, ammonium fluoride or ammonium bifluoride are used as corrosive agents, sodium sulfate is added to prepare roughening liquid, and the roughening liquid is used for carrying out corrosion treatment on glass fibers in the glass fiber reinforced plastic, so that the roughness of the glass fibers is increased, and the binding force between the glass fiber reinforced plastic and a coating is improved; meanwhile, fluoride salt is added to have synergistic effect with hydrogen fluoride, ammonium fluoride or ammonium bifluoride, so that the coarsening efficiency and the coarsening uniformity are improved. The components of the coarsening liquid are environment-friendly and non-toxic, and are favorable for sewage treatment and environmental protection.
Description
Technical Field
The invention relates to the technical field of electroplating, in particular to roughening liquid and a roughening method for roughening glass fiber reinforced plastic.
Background
The glass fiber reinforced plastic (glass fiber reinforced plastic for short) is a composite material with glass fiber and its product as reinforcing material and synthetic resin as base material. The glass fiber reinforced plastic can improve the strength and rigidity of the plastic material, reduce the thermal deformation of the plastic material, and improve the thermal deformation temperature of the plastic material, and the plastic and glass fiber materials are more and more widely used in the fields of automobiles and communication. Common glass fiber reinforced plastic materials include PP + glass fiber, PPs + glass fiber, PA66+ glass fiber, TPU + glass fiber, and the like. The glass fiber reinforced plastic has the characteristics of light weight, high strength, easy molding, corrosion resistance and the like, but has poor appearance effect and no luster. Therefore, the glass fiber reinforced plastic is usually electroplated to have a metallic luster, and the aging resistance, heat resistance, wear resistance and hardness of the glass fiber reinforced plastic are improved.
The common conventional process flow of glass fiber reinforced plastic electroplating comprises the following steps: surface finishing, cleaning, chemical roughening, cleaning, sensitizing, cleaning, distilled water washing, silver salt activation, cleaning, chemical copper plating, cleaning, electroplating thickening, cleaning, and other finishing or electroplating.
The coarsening is to dissolve the glass fiber in the material to form a pit, so that the surface of the glass fiber reinforced plastic forms a rough surface, and the binding force between the glass fiber reinforced plastic and the coating is improved. Therefore, the coarsening process is used as the most important part in the pretreatment process of electroplating, and is directly related to whether the glass fiber reinforced plastic and the plating layer have good bonding force.
Chinese patent No. CN200510012977.6 discloses a plastic electroplating chromic anhydride-sulfuric acid type roughening process, which comprises the following steps: (1) removing oil; (2) coarsening chromic anhydride-sulfuric acid; (3) recovering chromic anhydride, namely putting the roughened plating piece into a recovery tank to separate the carried chromic acid, and returning the chromic acid to the roughening tank for recycling; (4) three-stage closed water washing; (5) reduction; (6) and (4) rinsing in a countercurrent manner. The method can keep the coarsening solution in an optimal process range through chromic anhydride recovery and electrolysis, and ensures the coarsening quality of the plated part; and can recover chromic anhydride to the utmost extent without causing pollution.
Chinese patent No. CN201610163249.3 discloses a method for preparing a magnetic metal long fiber tube, wherein surface treatment of polypropylene continuous fibers is disclosed: chemical degreasing is respectively carried out by adopting a sodium hydroxide solution, the surfaces of chromic anhydride and sulfuric acid solution are roughened, acid tin salt solution is used for sensitizing fibers, silver nitrate and ammonia water solution are used for activating the surfaces of the fibers, and formaldehyde solution is used for reducing the fibers; electroless copper plating of the fibers, electroplating of the fibers (iron or nickel), removal of the polypropylene fibers, and reduction of the fiber metal tube.
Therefore, the traditional roughening process usually adopts sulfuric acid and chromic anhydride as roughening liquid for roughening, but the sulfuric acid and chromic anhydride-shaped roughening liquid has serious pollution, difficult maintenance, difficult sewage treatment and strong damage to the environment.
Disclosure of Invention
Aiming at the technical problems of large pollution, difficult maintenance, difficult sewage treatment and poor process binding force of the traditional sulfuric acid and chromic anhydride roughening solution at present. The roughening liquid for roughening the glass fiber reinforced plastic is environment-friendly, enhances the binding force between the substrate and the plating layer, has environment-friendly and non-toxic components, and is beneficial to sewage treatment and environment protection. The following specific technical scheme is adopted:
a roughening liquid for roughening glass fiber reinforced plastic is prepared from the following raw materials in concentration: 30-300ml/L of corrosive agent and 1-5g/L of sodium sulfate.
Preferably, the etchant is one of hydrogen fluoride, ammonium fluoride and ammonium bifluoride. The roughening liquid is mainly used for corroding and dissolving glass fibers in glass fiber reinforced plastic, and pits are formed in the surfaces of the glass fibers, so that the technical effect of improving the binding force between the glass fiber reinforced plastic and a coating is achieved. The corrosion resistance of the glass fiber is very good, so that one of hydrogen fluoride, ammonium fluoride and ammonium bifluoride is selected as the corrosive agent.
According to the invention, the glass fiber in the glass fiber reinforced plastic is corroded by using hydrogen fluoride, ammonium fluoride or ammonium bifluoride as a corrosive agent, the corrosion speed of the roughening solution on the glass fiber is further accelerated by adding sodium sulfate, and the production efficiency is improved.
Further, the coarsening liquid is prepared from the following raw materials in concentration: 30-300ml/L of corrosive agent, 1-3g/L of sodium sulfate and 8-12g/L of fluoride salt.
Preferably, the fluoride salt is one or more of magnesium fluoride, aluminum fluoride, calcium fluoride and potassium bifluoride. Through adding fluoride and corrosive agent synergism, on the one hand, reserve fluoride ion and improve the coarsening duration, and on the other hand, the fluoride can play a slow release effect, and prevents that the too fast corrosion rate from causing the coarsening nonuniform.
A coarsening method of glass fiber reinforced plastic comprises the following steps:
1) preparing a roughening liquid: adding purified water to half of the size of the tank body according to the size of the tank body, slowly adding the corrosive agent in the formula amount into the water, stirring continuously, adding the sodium sulfate and the fluoride salt in the formula amount, stirring uniformly, and adding the balance of water to obtain a coarsening liquid. Wherein the formula amounts of the corrosive agent, the sodium sulfate and the fluoride salt are as follows: 30-300ml/L of corrosive agent, 1-3g/L of sodium sulfate and 8-12g/L of fluoride salt;
2) roughening the workpiece pretreatment, which sequentially comprises: removing oil and washing;
3) heating the coarsening liquid to 30-45 ℃ by using a heating pipe;
4) roughening treatment: placing the pretreated coarsening workpiece into coarsening liquid, and stirring the coarsening liquid for 3-15 minutes;
5) and taking out the coarsened workpiece, washing with water, and drying.
Preferably, the specific method for removing oil in step 2) is to put the coarsened workpiece into an oil removing agent and soak the coarsened workpiece for 10 to 15 minutes at room temperature.
In one embodiment, the oil removing agent comprises 25-30g/L of sodium hydroxide solution, 15-20g/L of sodium carbonate solution, 10-15g/L of trisodium phosphate dodecahydrate solution and 3-5g/L of anionic polyacrylamide.
Preferably, the heating pipe in step 3) is a teflon heating pipe. The heating pipe made of the Teflon material can effectively prevent the heating pipe from being corroded by the roughening liquid in the using process.
Preferably, step 4) is carried out by stirring the roughening solution and simultaneously carrying out ultrasonic-assisted roughening on the roughening solution. Through the ultrasonic wave is supplementary, when improving alligatoring efficiency, improve the alligatoring degree of consistency.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention overcomes the technical problems of difficult coarsening maintenance and sewage treatment of the traditional sulfuric acid and chromic anhydride, adopts hydrogen fluoride, ammonium fluoride or ammonium bifluoride as a corrosive agent, and adds sodium sulfate to prepare the coarsening liquid, and the coarsening liquid has environment-friendly and non-toxic components, and is beneficial to sewage treatment and environmental protection.
2. The coarsening liquid mainly carries out corrosion treatment on glass fibers in the glass fiber reinforced plastic, and increases the roughness of the glass fibers so as to improve the bonding force between the glass fiber reinforced plastic and the plating layer; meanwhile, fluoride salt is added to have synergistic effect with hydrogen fluoride, ammonium fluoride or ammonium bifluoride, so that the coarsening efficiency and the coarsening uniformity are improved.
Drawings
FIG. 1 is a photograph of a sample of the workpiece after the degreasing treatment in example 3.
FIG. 2 is a photograph of a sample of the roughened workpiece of example 3.
FIG. 3 is a photograph of a sample of the nickel-plated workpiece of example 3
Detailed Description
The present invention will be described in further detail by way of specific embodiments, but it should not be construed that the scope of the present invention is limited to the following examples. Various substitutions and alterations can be made by those skilled in the art and ordinary skill in the art without departing from the spirit of the method of the invention described above.
Example 1
A coarsening method of glass fiber reinforced plastic comprises the following steps:
1) preparing a roughening liquid: adding purified water to half of the size of the tank body according to the size of the tank body, slowly adding 150ml/L hydrogen fluoride into the water, stirring continuously, adding 1g/L sodium sulfate, stirring uniformly, and adding the balance of water to obtain a coarsening liquid.
2) And (3) placing the coarsened workpiece into a degreasing agent, and soaking for 15 minutes at room temperature, wherein the degreasing agent comprises 30g/L of sodium hydroxide solution, 20g/L of sodium carbonate solution, 15g/L of trisodium phosphate dodecahydrate solution and 5g/L of anionic polyacrylamide.
3) The roughening solution was heated to 40 ℃ using Teflon.
4) Roughening treatment: placing the pretreated coarsening workpiece into coarsening liquid, and stirring the coarsening liquid for 15 minutes;
5) and taking out the coarsened workpiece, and washing and drying the workpiece.
Example 2
A coarsening method of glass fiber reinforced plastic comprises the following steps:
1) preparing a roughening liquid: adding purified water to half of the size of the tank body according to the size of the tank body, slowly adding 200ml/L ammonium fluoride into the water, stirring continuously, adding 3g/L sodium sulfate, stirring uniformly, and adding the balance of water to obtain a coarsening liquid.
2) And (3) placing the coarsened workpiece into a degreasing agent, and soaking for 15 minutes at room temperature, wherein the degreasing agent comprises 30g/L of sodium hydroxide solution, 20g/L of sodium carbonate solution, 15g/L of trisodium phosphate dodecahydrate solution and 5g/L of anionic polyacrylamide.
3) The coarsening liquid is heated to 40 ℃ by using a Teflon heating tube.
4) Roughening treatment: placing the pretreated coarsening workpiece into coarsening liquid, stirring the coarsening liquid, and simultaneously carrying out ultrasonic assistance on the groove body through an ultrasonic vibrator for 15 minutes;
5) and taking out the coarsened workpiece, and washing and drying the workpiece.
Example 3
A coarsening method of glass fiber reinforced plastic comprises the following steps:
1) preparing a roughening liquid: adding purified water to half of the size of the tank body according to the size of the tank body, slowly adding 300ml/L of hydrogen fluoride into the water, stirring continuously, adding 3g/L of sodium sulfate and 8g/L of magnesium fluoride, stirring uniformly, and adding the balance of water to obtain a coarsening liquid.
2) And (3) placing the coarsened workpiece into a degreasing agent, and soaking for 15 minutes at room temperature, wherein the degreasing agent comprises 30g/L of sodium hydroxide solution, 20g/L of sodium carbonate solution, 15g/L of trisodium phosphate dodecahydrate solution and 5g/L of anionic polyacrylamide.
3) The roughening solution was heated to 40 ℃ using Teflon.
4) Coarsening treatment: placing the pretreated coarsening workpiece into coarsening liquid, stirring the coarsening liquid, and simultaneously carrying out ultrasonic assistance on the tank body through an ultrasonic vibrator for 15 minutes;
5) and taking out the coarsened workpiece, and washing and drying the workpiece.
Example 4
A coarsening method of glass fiber reinforced plastic comprises the following steps:
1) preparing a roughening liquid: adding purified water to half of the size of the tank body according to the size of the tank body, slowly adding 250ml/L ammonium bifluoride into the water, stirring continuously, adding 2g/L sodium sulfate and 9g/L potassium bifluoride, stirring uniformly, and adding the balance of water to obtain a coarsening liquid.
2) And (3) placing the coarsened workpiece into a degreasing agent, and soaking for 15 minutes at room temperature, wherein the degreasing agent comprises 30g/L of sodium hydroxide solution, 20g/L of sodium carbonate solution, 15g/L of trisodium phosphate dodecahydrate solution and 5g/L of anionic polyacrylamide.
3) The roughening solution was heated to 40 ℃ using Teflon.
4) Coarsening treatment: placing the pretreated coarsening workpiece into coarsening liquid, stirring the coarsening liquid, and simultaneously carrying out ultrasonic assistance on the groove body through an ultrasonic vibrator for 15 minutes;
5) and taking out the coarsened workpiece, and washing and drying the workpiece.
Comparative example 1
The method comprises the following steps of (1) carrying out coarsening treatment on a workpiece by adopting a plastic electroplating chromic anhydride-sulfuric acid type coarsening process with the application number of CN200510012977.6, wherein the method specifically comprises the following steps: (1) acid oil removal and oil removal liquid composition: chromic anhydride 400g/L and sulfuric acid 400g/L, soaking for 10 minutes at room temperature; (2) coarsening, wherein the composition of a coarsening liquid is as follows: 400g/L of chromic anhydride and 400g/L of sulfuric acid, coarsening for 10 minutes at 70 ℃ under the condition of air stirring, and arranging a trivalent chromium electrolysis device in a coarsening tank; (3) and (5) three-stage closed water washing.
And (3) experimental comparison:
the coarsening work pieces obtained in the embodiments 1-5 and the comparative example 1 of the invention are chemically plated with nickel according to the traditional plastic electroplating process, and the specific process is that the coarsening work pieces are immersed into the mixed solution of 50g/l hydrochloric acid and 0.01g/l palladium chloride for activation treatment, and are taken out for washing after 2 minutes; and (3) putting the thick washed workpiece into a nickel plating solution with the temperature of 80 ℃, nickel sulfate of 1mol/l, sodium hypophosphite of 0.2mol/l and sodium succinate of 0.1mol/l for nickel plating, taking out the workpiece after reaching the required thickness of the nickel metal plating layer, washing with water and drying to obtain a finished product of the nickel-plated workpiece.
Carrying out a check test on a finished product of a nickel-plated workpiece, and testing the coating binding force of the finished product, wherein the specific method comprises the following steps: and (3) scratching 12 orthogonal scratches on the surface of the coating by using a special testing cutting knife, wherein the scratches penetrate through the paint film, the distance between every two adjacent scratches is 2mm, forming a 5X 5 grid, and applying a special adhesive tape to carry out 180-degree stripping test.
Tests show that the combination force of the work piece roughened by the roughening method and the plating layer is high, and the effect of roughening the work piece by adopting a chromic anhydride-sulfuric acid type roughening process can be achieved. But compared with a chromic anhydride-sulfuric acid type coarsening process, the coarsening liquid has the advantages of environment-friendly and non-toxic components, and is beneficial to sewage treatment and environmental protection.
The test results are recorded as follows:
Claims (5)
1. the roughening liquid for roughening the glass fiber reinforced plastic is characterized by comprising the following raw materials:
300ml/L of caustic agent 150-;
the corrosive agent is hydrogen fluoride;
the fluoride salt is one or a mixture of magnesium fluoride, aluminum fluoride, calcium fluoride and potassium bifluoride.
2. The coarsening method of the glass fiber reinforced plastic is characterized by comprising the following steps:
1) preparing a roughening liquid: adding purified water to half of the size of the tank body according to the size of the tank body, and slowly adding the corrosive agent in the formula amount
Adding water, continuously stirring, adding sodium sulfate and fluoride salt according to the formula, uniformly stirring, and adding the balance of water to obtain a coarsening solution;
the corrosive agent is hydrogen fluoride;
the fluoride salt is one or a mixture of magnesium fluoride, aluminum fluoride, calcium fluoride and potassium bifluoride;
the formula amount is as follows: 300ml/L of corrosive agent 150-;
2) roughening the workpiece pretreatment, which sequentially comprises: removing oil and washing;
3) heating the coarsening liquid to 30-45 ℃ by using a heating pipe;
4) roughening treatment: placing the pretreated coarsening workpiece into coarsening liquid, and stirring the coarsening liquid for 3-15 minutes;
5) and taking out the coarsened workpiece, and washing and drying the workpiece.
3. The method for roughening glass fiber reinforced plastic as claimed in claim 2, wherein the degreasing step in step 2)
The specific method comprises the steps of putting a coarsened workpiece into an oil removing agent, soaking for 10-15 minutes at room temperature, wherein the oil removing agent comprises the following components
25-30g/L of sodium hydroxide solution, 15-20g/L of sodium carbonate solution and 10-15g/L of trisodium phosphate dodecahydrate solution
And 3-5g/L of anionic polyacrylamide.
4. The method for roughening glass fiber reinforced plastic as claimed in claim 2, wherein the heating in step 3) is performed
The tube is a Teflon heating tube.
5. The method for roughening glass fiber reinforced plastic as claimed in claim 2, wherein step 4) is roughening by stirring
And simultaneously carrying out ultrasonic-assisted roughening on the roughening liquid.
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| CN111748806A (en) * | 2020-07-21 | 2020-10-09 | 江苏悦锌达新材料有限公司 | Roughening liquid for polyphenylene sulfide and composite material thereof, preparation method and use method thereof |
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| GB1151542A (en) * | 1966-06-09 | 1969-05-07 | Chemical And Aerospace Product | Method for Etching Glass Reinforced Plastics |
| DE3680699D1 (en) * | 1985-04-11 | 1991-09-12 | Olin Hunt Sub Iii Corp | METHOD FOR PREPARING A CONDUCTIVE CARRIER FOR ELECTROPLATING. |
| CN1195099C (en) * | 1998-07-07 | 2005-03-30 | 株式会社日矿材料 | Pretreating agent for metal plating, and method for metal plating using same |
| CN101792923A (en) * | 2010-04-14 | 2010-08-04 | 上海交通大学 | Method for titanium plate surface nanoscale roughening |
| CN104761150B (en) * | 2015-03-16 | 2017-09-22 | 南昌欧菲光学技术有限公司 | Glass etching liquid, the method using etching solution etching glass, cover-plate glass and preparation method thereof |
| US10804111B2 (en) * | 2015-09-15 | 2020-10-13 | Nissan Chemical Industries, Ltd. | Method for roughening surface using wet treatment |
| CN109020252A (en) * | 2018-09-19 | 2018-12-18 | 安徽宇臻实业有限公司 | A kind of glass etching formula of liquid |
| CN109402708B (en) * | 2018-10-17 | 2020-04-24 | 中国兵器工业第五九研究所 | Preparation method of aluminum and aluminum alloy wear-resistant self-lubricating coating |
| CN112048745A (en) * | 2020-09-16 | 2020-12-08 | 广东博迅通信技术有限公司 | Process for improving binding force between metalized coating on surface of plastic vibrator and plastic base material and improving PIM value of coating |
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