CN109137047B - A kind of method for preparing latex film by electrodeposition on metal surface - Google Patents

Abstract

The present invention provides a method for preparing a latex film by electro-deposition on a metal surface, which can be either non-electrical or electrified. At room temperature, two metals are connected together without electricity, and then placed in the tank of 906 emulsion or the self-made PVAc emulsion of the present invention, and after drying, a latex film is prepared on the surface of the negative electrode metal. Alternatively, a latex film can be rapidly prepared on the anodic metal electrode by electro-deposition at room temperature with the power switched on. By changing the type of emulsion and adjusting the deposition time and voltage, the thickness of the latex film can be precisely controlled, and a layer of latex film with a thickness of 9–620 μm is obtained at the anode. The latex film is prepared on the metal electrode of the present invention, and the metal with the latex film is bonded, and it does not need to be placed in the air for a long time to complete the film-forming process of volatilization of moisture, the film-forming speed is fast, and the film-forming time is effectively saved. Increase productivity. The raw material of the invention is easy to obtain, the process is simple, the cost is low, the conditions are mild and environmentally friendly, and the body of the operator is not harmed.

Description

A kind of method for preparing latex film by electrodeposition on metal surface

technical field

The invention belongs to the technical field of polymer preparation, and relates to a method for preparing a latex film by electro-deposition on a metal surface.

Background technique

Traditional emulsion film making methods include spraying, coating, dipping and so on. However, these emulsion film-making methods have some common and difficult-to-solve problems. The emulsions have the following problems during curing: it is difficult to coat evenly on non-planar surfaces; it is difficult to adjust the thickness of the film, and it is difficult to precisely control the coating amount, which affects the The film thickness affects the function; after sizing, the emulsion needs to be placed in the air for a long time to complete the volatilization process of water, and it cannot form a film quickly. Moreover, it is difficult to apply the emulsion evenly on the irregular metal surface; secondly, the film formation by these methods must go through the process of drying and film formation, which is often accompanied by the formation of shells, edge effects, microbubbles and other phenomena, which seriously affect the The morphology, performance, etc. of the film formation; finally, these methods have a slow film formation speed, which is not an example for practical applications.

SUMMARY OF THE INVENTION

In order to solve the problems existing in the prior art, the present invention provides a method for preparing a latex film by electro-deposition on a metal surface.

The Chinese name of the relevant abbreviations of the present invention: PVAc is polyvinyl acetate emulsion, PVA is polyvinyl alcohol, OP-10 is polyoxyethylene octyl phenol ether-10, SDS is sodium dodecyl sulfonate, KPS is persulfuric acid Potassium, VAc is vinyl acetate, DBP is dibutyl phthalate. 906 is an acrylic tackifying emulsion.

A method for preparing a latex film by electro-deposition on a metal surface provided by the present invention, the steps and conditions are as follows:

Emulsion used is 906 emulsion, there is commodity on the market, or the PVAc emulsion that is self-made of the present invention;

About 906 Emulsion: 906 Emulsion is polyurethane acrylate RE-906 PUA tackifying emulsion, 906 Emulsion has a pH value of 4.0–7.0, a viscosity of 300–1000 mps, and a solids content of 52.0±2.0;

(1) Preparation of PVAc emulsion

1.1 At room temperature, put PVA and deionized water in a four-port reactor at a mass ratio of 1:9, and heat and dissolve at 90 °C to obtain a PVA solution with a mass concentration of 10%;

1.2 Then press the mass of the PVA solution with a mass concentration of 10% g: the mass of PVA g: the mass of deionized water g: the volume of OP-10 mL: the mass of SDS g: the volume of KPS solution mL: the volume of VAc in mL is 30 : 9: 12: 0.8: 0.25: 2: 5, the last 6 raw materials were added to the PVA solution in turn, the mass volume concentration of KPS was 10 mg/mL, and the reaction was refluxed and stirred in a water bath at 70 °C for 1 h. , to obtain a reaction solution;

1.3 According to the mass of the obtained PVA solution with a mass concentration of 10%, g: the volume of VAc in mL: the volume of KPS in mL is 30:27:6, and VAc and KPS are added dropwise to the reaction solution alternately, within 2 h. After finishing, the mass volume concentration of KPS is 10mg/mL;

1.4 Next, heat up to 90 °C, react to no reflux, then cool to 50 °C, adjust the pH to 5, and add DBP according to the mass ratio of the obtained PVA solution with a mass concentration of 10%: DBP 30:9, and react for 30 min. Obtain PVAc emulsion;

(2) Preparation of latex film on metal surface by electrodeposition method

At room temperature, two metal electrodes were placed in a tank containing 906 emulsion or self-made PVAc emulsion, and the two metal electrodes were separated by 1 cm, without electricity or electricity, and the latex film was prepared on the cathode metal surface by electro-deposition method.

2.1 At room temperature, connect the two metals together without electricity, and then place them in the 906 emulsion purchased above or the PVAc emulsion made by the present invention, and the two metals are separated by 1 cm. After 3600 s, take out and rinse with deionized water. After drying, a latex film is prepared on the surface of the negative metal;

2.2 At room temperature, place two metal electrodes in the tank containing the purchased 906 emulsion or prepared PVAc emulsion, with a distance of 1 cm between the two metal electrodes, turn on the power supply, adjust the power supply voltage to 0.5–15 V, and the power-on time For 5–6000 s, then power off, take out the electrode to rinse, and after drying, a latex film with a thickness of 9–620 μm is obtained on the surface of the anode metal.

The metal electrode is preferably iron, copper, zinc or aluminum.

The bonding method of the latex film prepared by the electro-deposition method: at room temperature, the two metals deposited with the electro- latex film are taken out from the latex and directly bonded, and a continuous force of 0.15 MPa is applied for 1 min to make the two metals. The metals were bonded together, and the samples were firmly bonded after 12 h.

Beneficial effects: The method for preparing a latex film by electro-deposition on a metal surface provided by the present invention has the following advantages: a method that is not electrified or electrified can be used. At room temperature, two metals are connected together without electricity, and then placed in the tank of 906 emulsion or the self-made PVAc emulsion of the present invention, and after drying, a latex film is prepared on the surface of the negative electrode metal. Alternatively, at room temperature, the power supply can be turned on, and the latex film can be quickly prepared on the electro-metal electrode by the electro-deposition method. By changing the type of the latex, adjusting the deposition time and voltage, the thickness of the latex film can be precisely controlled, and a layer of the anode metal surface can be obtained. Latex films with a thickness of 9–620 μm. The latex film is prepared on the metal electrode of the present invention, and the metal with the latex film is bonded, and it does not need to be placed in the air for a long time to complete the film-forming process of volatilization of moisture, the film-forming speed is fast, and the film-forming time is effectively saved. Increase productivity. The raw material of the invention is easy to obtain, the process is simple, the cost is low, the conditions are mild and environmentally friendly, and the body of the operator is not harmed.

Detailed ways

Example 1 A method for preparing a latex film by electro-deposition on a metal surface, the latex is 906 latex, purchased from Sihui Bangdeli Chemical Co., Ltd. The steps and conditions are as follows:

At room temperature, metal copper with a diameter of 0.8 mm and metal zinc with a diameter of 0.5 mm are connected together without electricity, and then placed in the 906 emulsion purchased above, the two metals are separated by 1 cm, and taken out after 3600 s. After rinsing with ionized water and drying, a latex film with a thickness of 54 μm was prepared on the surface of the negative metal zinc. The electrode diameter had no effect on the prepared latex films.

The bonding method of the latex film prepared by the electro-deposition method: at room temperature, the two metals deposited with the electro- latex film are taken out from the latex, and the end faces are directly bonded, and a continuous force of 0.15 MPa is applied for 1 min to make The two metals were bonded together and the bond strength was measured to be 0.012 MPa after drying.

Example 2 A method for preparing a latex film by electro-deposition on a metal surface, the latex is 906 latex, purchased from Sihui Bangdeli Chemical Co., Ltd. The steps and conditions are as follows:

At room temperature, two iron electrodes with a diameter of 0.75 mm were placed in the 906 emulsion with an interval of 1 cm, and the power was turned on, the power supply voltage was set to 0.5 V, and the power-on time was 60 s. After that, a latex film with a thickness of 18 μm was obtained on the surface of the anode metal.

The bonding method of the latex film prepared by the electro-deposition method: at room temperature, the two metals deposited with the electro- latex film are taken out from the latex, and the end faces are directly bonded, and a continuous force of 0.15 MPa is applied for 1 min to make The two metals were bonded together and the bond strength was measured to be 0.045 MPa after drying.

Example 3 A method for preparing a latex film by electro-deposition on a metal surface, the latex is 906 latex, purchased from Sihui Bangdeli Chemical Co., Ltd. The steps and conditions are as follows:

(1) Electrodeposition method to prepare latex film

At room temperature, two iron electrodes with a diameter of 0.75 mm were placed in the 906 emulsion, separated by 1 cm, and the power was turned on, the power supply voltage was set to 15 V, and the power-on time was 6000 s. Afterwards, a latex film with a thickness of 292 μm was obtained on the surface of the anode metal.

The bonding method of the latex film prepared by the electro-deposition method: at room temperature, the two metals deposited with the electro- latex film are taken out from the latex, and the end faces are directly bonded, and a continuous force of 0.15 MPa is applied for 1 min to make The two metals were bonded together and the bond strength was measured to be 0.056 MPa after drying.

Example 4 A method for preparing a latex film by electro-deposition on a metal surface, the latex is 906 latex, purchased from Sihui Bangdeli Chemical Co., Ltd. The steps and conditions are as follows:

Two zinc electrodes with a thickness of 0.1 mm, a width of 0.5 cm, and a length of 5 cm were placed in the 906 emulsion at room temperature, and the two metal electrodes were separated by 1 cm. The power was turned on, the power supply voltage was adjusted to 8 V, and the power-on time was 300 s. After the power was turned off, a latex film with a thickness of 230 μm was obtained on the surface of the anode metal zinc.

The bonding method of the electro-emulsion film: at room temperature, the two metal zinc electrodes deposited with the electro-emulsion film were taken out from the emulsion and directly bonded. The contact area was 0.5*0.5 cm ² , and a continuous The force was applied for 1 min to bond the two metal zinc blocks together, and the bond strength was measured to be 2.24 MPa after drying.

Example 5 A method for preparing a latex film by electro-deposition on a metal surface, the latex is 906 latex, purchased from Sihui Bangdeli Chemical Co., Ltd. The steps and conditions are as follows:

At room temperature, an aluminum wire mesh with a pore size of 1.6 mm*1.6 mm, a diameter of 0.35 mm, and a length of 2 cm was used as the anode, and a cylindrical iron wire with a diameter of 0.75 mm was used as the cathode. Turn on the power supply, set the power supply voltage to 8 V, and set the power-on time to 180 s. Take out the electrode and rinse it in deionized water. After drying, a latex film with a thickness of 180 μm is obtained on the surface of the anode aluminum metal.

Example 6 A method for preparing a latex film by electro-deposition on a metal surface, the latex is 906 latex, purchased from Sihui Bangdeli Chemical Co., Ltd., the steps and conditions are as follows:

At room temperature, copper with a diameter of 0.8 mm was used as the anode and aluminum with a diameter of 1 mm was used as the cathode, placed in the 906 emulsion with an interval of 1 cm, and the power was turned on. The electrode was rinsed in deionized water, and after drying, a latex film with a thickness of 60 μm was obtained on the surface of the anode copper metal.

The bonding method of the latex film prepared by the electro-deposition method: at room temperature, the two metals deposited with the electro- latex film are taken out from the latex, and the end faces are directly bonded, and a continuous force of 0.15 MPa is applied for 1 min to make The two metals were bonded together and the bond strength was measured to be 0.057 MPa after drying.

Example 7 A method for preparing a latex film by electro-deposition on a metal surface, the emulsion is a self-made PVAc emulsion, and the steps and conditions are as follows:

(1) Preparation of PVAc emulsion

1.1 At room temperature, first place 3g of PVA and 27g of deionized water in a 250 mL four-necked flask, heat and dissolve at 90 °C to obtain a PVA solution;

1.2 Add 12 mL of deionized water, 0.8 mL of OP-10, 0.25 g of SDS, 2 mL of KPS solution with a mass/volume concentration of 10 mg/mL, and 5 mL of VAc in sequence, and reflux and stir in a water bath at 70 °C The reaction was carried out for 1 h to obtain a reaction solution;

1.3 27 mL of VAc and 6 mL of KPS with a mass-volume concentration of 10 mg/mL were added alternately to the reaction solution, and the addition was completed dropwise within 2 h;

1.4 Next, heat up to 90 °C, react to no reflux, then cool to 50 °C, adjust the pH to 5, and finally add 9 g of DBP and react for 30 min to obtain PVAc emulsion;

(2) Preparation of latex film by electrodeposition method

At room temperature, two iron electrodes with a diameter of 0.75 mm were placed in the tank containing the PVAc emulsion prepared above, and the two metal electrodes were separated by 1 cm. The power was turned on, the power supply voltage was adjusted to 8 V, and the power-on time was 5 s. Then power off, take out the electrode and rinse it in deionized water. After drying, a latex film with a thickness of 9 μm is obtained on the surface of the anode metal.

The bonding method of the latex film prepared by the electro-deposition method: at room temperature, the two metals deposited with the electro- latex film are taken out from the latex, and the end faces are directly bonded, and a continuous force of 0.15 MPa is applied for 1 min to make The two metals were bonded together and the bond strength was measured to be 0.025 MPa after drying.

Example 8 A method for preparing a latex film by electro-deposition on a metal surface, the emulsion is a self-made PVAc emulsion, and the steps and conditions are as follows:

(1) Preparation of PVAc emulsion, same as Example 7.

(2) The latex film was prepared by the electro-deposition method, the electrification time was 600 s, the thickness of the latex film prepared on the surface of the anode metal was 620 μm, and the rest were the same as in Example 7.

Example 9 A method for preparing a latex film by electro-deposition on a metal surface, the emulsion is a self-made PVAc emulsion, and the steps and conditions are as follows:

(1) Preparation of PVAc emulsion, same as Example 7.

(2) The latex film was prepared by electro-deposition method: at room temperature, two zinc electrodes with a thickness of 0.1 mm, a width of 0.5 cm, and a length of 5 cm were placed in the PVAc emulsion, and the two metal electrodes were separated by 1 cm. The power supply voltage was adjusted to 8 V, the power-on time was 300 s, and then the power was turned off, and the thickness of the latex film prepared on the surface of the anode zinc metal was 330 μm.

The bonding method of the electro-emulsion film: at room temperature, the two metal zinc electrodes deposited with the electro-emulsion film were taken out from the emulsion and directly bonded. The contact area was 0.5*0.5 cm ² , and a continuous The force was applied for 1 min to bond the two metal zinc blocks together, and the bond strength was measured to be 2.33 MPa after drying.

Example 10 A method for preparing a latex film by electro-deposition on a metal surface, the emulsion is a self-made PVAc emulsion, and the steps and conditions are as follows:

At room temperature, metal copper with a diameter of 0.8 mm and metal zinc with a diameter of 0.5 mm were connected together without electricity, and then placed in a homemade PVAc emulsion, the two metals were separated by 1 cm, and taken out after 3600 s with deionization After rinsing with water and drying, a latex film with a thickness of 98 μm was prepared on the surface of the negative metal zinc.

The bonding method of the latex film prepared by the electro-deposition method: at room temperature, the two metals deposited with the electro- latex film are taken out from the latex, and the end faces are directly bonded, and a continuous force of 0.15 MPa is applied for 1 min to make The two metals were bonded together and the bond strength was measured to be 0.011 MPa after drying.

Claims (7)

1. A method for preparing a latex film on a metal surface by electrodeposition is characterized by comprising the following steps and conditions:

the emulsion used is 906 emulsion, commercially available on the market, or a self-made PVAc emulsion;

with respect to the 906 emulsion: the 906 emulsion is polyurethane acrylate RE-906PUA tackifying emulsion, the pH value of the 906 emulsion is 4.0-7.0, the viscosity is 300-1000 mps, and the solid content is 52.0 +/-2.0;

(1) preparation of PVAc emulsion

1.1 at room temperature, firstly, putting PVA and deionized water in a four-port reactor according to the mass ratio of 1:9, and heating and dissolving at 90 ℃ to obtain a PVA solution with the mass concentration of 10%;

1.2 adding the last 6 raw materials into the PVA solution in sequence according to the mass g of the PVA solution with the mass concentration of 10%, the mass g of the PVA, the mass g of deionized water, OP-10 volume m L, the mass g of SDS, the volume m L of KPS solution and the volume m L of VAc, which are 30: 9: 12: 0.8: 0.25: 2: 5, wherein the mass volume concentration of the KPS solution is 10mg/m L, and carrying out reflux stirring reaction in a water bath at 70 ℃ for 1h to obtain a reaction solution;

1.3, alternately dropwise adding the VAc solution and the KPS solution into the reaction solution within 2h according to the mass g of the obtained PVA solution with the mass concentration of 10%, the volume m L of the VAc solution and the volume m L of the KPS solution of 30: 27: 6, wherein the mass volume concentration of the KPS solution is 10mg/m L;

1.4 the temperature is then raised to 90 ℃, the reaction is carried out until no reflux exists, then the reaction product is cooled to 50 ℃, the pH value is adjusted to 5, and the PVA solution with the mass concentration of 10 percent is obtained: the mass ratio of DBP is 30: 9, adding the PVA into DBP, and reacting for 30min to prepare PVAc emulsion;

(2) preparing emulsion film on metal surface by using electrodeposition method

Placing two metal electrodes in a tank containing 906 emulsion or prepared PVAc emulsion at room temperature, wherein the interval between the two metal electrodes is 1cm, and preparing an emulsion film on the surface of the anode metal when electrifying; or when the power is not supplied, preparing an emulsion film on the metal surface of the negative electrode.

2. The method for preparing a latex film on a metal surface by electrodeposition according to claim 1, wherein the method for applying current comprises the following steps and conditions:

and (2) at room temperature, placing two metal electrodes in a tank containing 906 emulsion or self-made PVAc emulsion, wherein the interval between the two metal electrodes is 1cm, switching on a power supply, adjusting the power supply voltage to be 0.5-15V, switching on for 5-6000 s, then switching off the power supply, taking out the electrodes, rinsing, drying, and obtaining a layer of emulsion film on the surface of the anode metal.

3. The method for preparing a latex film on a metal surface by electrodeposition according to claim 2, wherein the method for applying current comprises the following steps and conditions: the power supply voltage is adjusted to be 8V, and the power-on time is 5 s.

4. The method for preparing a latex film on a metal surface by electrodeposition according to claim 2, wherein the method for applying current comprises the following steps and conditions: the voltage of the power supply is adjusted to be 8V, and the power-on time is 300 s.

5. The method for preparing a latex film on a metal surface by electrodeposition according to claim 2, wherein the method for applying current comprises the following steps and conditions: the voltage of the power supply is adjusted to be 8V, and the power-on time is 600 s.

6. The method of claim 1, wherein the step of applying no electrical power comprises the following steps and conditions:

connecting two metals together at room temperature, not electrifying, then putting the two metals into the purchased 906 emulsion or the self-made PVAc emulsion, separating the two metals by 1cm, taking out after 3600s, rinsing the two metals by using deionized water, drying the two metals, and preparing the emulsion film on the surface of the negative electrode metal.

7. The method of claim 1 or 2, wherein the metal is iron, copper, zinc or aluminum.