CN111455414A - Additive for producing gradual change type electrolytic copper foil - Google Patents
Additive for producing gradual change type electrolytic copper foil Download PDFInfo
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- CN111455414A CN111455414A CN202010159229.5A CN202010159229A CN111455414A CN 111455414 A CN111455414 A CN 111455414A CN 202010159229 A CN202010159229 A CN 202010159229A CN 111455414 A CN111455414 A CN 111455414A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D1/00—Electroforming
- C25D1/04—Wires; Strips; Foils
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/38—Electroplating: Baths therefor from solutions of copper
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Abstract
The invention discloses an additive for producing a gradual change type electrolytic copper foil, which is prepared from the following raw materials in parts by weight: 30-120 parts of chlorine-containing compound, 10-150 parts of polyether compound, 50-600 parts of collagen, 30-600 parts of sodium polydithio-dipropyl sulfonate, 10-200 parts of polyethylene glycol, 20-500 parts of 2-mercapto benzimidazole, 10-600 parts of ethylene thiourea and 10-200 parts of tetrahydrothiazole thioketone, wherein the molecular weight of the polyether compound is 4000-20000, and the molecular weight of the polyethylene glycol is 6000-10000. The invention also provides a preparation method of the additive, which comprises the step of adding metered chlorine-containing compounds, polyether compounds, collagen, sodium polydithio-dipropyl sulfonate, polyethylene glycol, 2-mercapto benzimidazole, ethylene thiourea and thiazolidinethione into the copper sulfate solution. The invention can improve the surface hardness of the electrolytic copper foil and prolong the maintenance time of the surface hardness, and effectively solves the problems that the electrolytic copper foil is soft, wrinkles are easy to generate in the production process of downstream manufacturers, the yield of the downstream manufacturers is reduced, and the production cost is increased.
Description
Technical Field
The invention relates to the technical field of electrolytic copper foil, in particular to an additive of electrolytic copper foil, and especially relates to an additive for producing a gradient electrolytic copper foil.
Background
The electrolytic copper foil is an important material for manufacturing copper clad laminates (CC L), Printed Circuit Boards (PCBs) and lithium ion batteries, in the high-speed development of the current electronic information industry, the electrolytic copper foil is called a 'neural network' for signal and power transmission and communication of electronic products, 2002, the production value of the printed circuit boards in China has gone beyond the third position in the world, and the copper clad laminates serving as substrate materials of the PCBs are also the third largest producing country in the world.
Currently, the mainstream electrolytic copper foil used for the negative current collector of the lithium ion battery is generally 5-8 microns thick, but the problem of copper foil warping often occurs in the production process, and firstly, the slitting quality of the copper foil is influenced; secondly, copper foil wrinkles are easily caused; thirdly, when the copper foil is coated as a current collector, cracks are easily caused between the active electrode material and the copper foil. Particularly, in the second place, the copper foil wrinkles seriously affect the downstream processing efficiency and quality. However, in the prior art, the mechanical strength of the copper foil is affected by the low surface hardness of the electrolytic copper foil. When the surface hardness of the copper foil is increased, the elongation of the copper foil is lowered, and the surface hardness is maintained for a short time, generally about 12 hours. The wrinkles are easily generated in the production process of downstream manufacturers, the yield of the downstream manufacturers is reduced, and the production cost is increased.
Disclosure of Invention
The invention provides an additive for producing a gradient electrolytic copper foil, which effectively improves the surface hardness of the electrolytic copper foil, prolongs the time for maintaining the surface hardness, avoids the wrinkle of the copper foil, improves the yield of downstream processes and reduces the production cost.
In order to solve the technical problems, the technical scheme of the invention is as follows:
an additive for producing a graded electrolytic copper foil: the material is prepared from the following raw materials in parts by weight: 30-120 parts of chlorine-containing compound, 10-150 parts of polyether compound, 50-600 parts of collagen, 30-600 parts of sodium polydithiodipropyl sulfonate, 10-200 parts of polyethylene glycol, 20-500 parts of 2-mercaptobenzimidazole, 10-600 parts of ethylene thiourea and 10-200 parts of tetrahydrothiazolethione, wherein the molecular weight of the polyether compound is 4000-20000, and the molecular weight of the polyethylene glycol is 6000-10000.
Preferably, the feed additive is prepared from the following raw materials in parts by weight: 30-100 parts of chlorine-containing compound, 10-100 parts of polyether compound, 50-300 parts of collagen, 30-400 parts of sodium polydithio-dipropyl sulfonate, 10-100 parts of polyethylene glycol, 20-300 parts of 2-mercapto benzimidazole, 10-400 parts of ethylene thiourea and 10-80 parts of tetrahydrothiazole thioketone, wherein the molecular weight of the polyether compound is 4000-10000, and the molecular weight of the polyethylene glycol is 6000-8000.
Preferably, the feed additive is prepared from the following raw materials in parts by weight: 100-120 parts of chlorine-containing compound, 100-150 parts of polyether compound, 300-600 parts of collagen, 400-600 parts of sodium polydithio-dipropyl sulfonate, 100-200 parts of polyethylene glycol, 300-500 parts of 2-mercapto benzimidazole, 400-600 parts of ethylene thiourea and 80-200 parts of tetrahydrothiazole thione, wherein the molecular weight of the polyether compound is 10000-20000, and the molecular weight of the polyethylene glycol is 8000-10000.
More preferably, the feed additive is prepared from the following raw materials in parts by weight: 80-110 parts of chlorine-containing compound, 50-120 parts of polyether compound, 200-400 parts of collagen, 450 parts of sodium polydithio-dipropyl sulfonate, 50-150 parts of polyethylene glycol, 400 parts of 2-mercapto benzimidazole, 300 parts of ethylene thiourea and 50-150 parts of tetrahydrothiazole thioketone, wherein the molecular weight of the polyether compound is 8000-18000, and the molecular weight of the polyethylene glycol is 8000-10000.
Particularly preferably, the compound is prepared from the following raw materials in parts by weight: 100 parts of chlorine-containing compound, 100 parts of polyether compound, 300 parts of collagen, 400 parts of sodium polydithio-dipropyl sulfonate, 100 parts of polyethylene glycol, 300 parts of 2-mercapto benzimidazole, 500 parts of ethylene thiourea and 120 parts of thiazolidinethione, wherein the molecular weight of the polyether compound is 16000, and the molecular weight of the polyethylene glycol is 8000.
Preferably, the molecular formula of the 2-mercaptobenzimidazole is C7H6N 2S; the molecular formula of the ethylene thiourea is C3H6N 2S; the molecular formula of the thiazolidinethione is C3H5NS 2.
The structural formula of the 2-mercaptobenzimidazole (C7H6N2S) is as follows:
the structural formula of the ethylene thiourea (C3H6N2S) is as follows:
the structural formula of the thiazolidinethione (C3H5NS2) is as follows:
collagen is a family of proteins, and at least over 30 genes encoding collagen chains have been found, and it can form more than 16 kinds of collagen molecules, and can be classified into fibrous collagen, basement membrane collagen, microfibril collagen, anchored collagen, hexagonal network collagen, non-fibrous collagen, transmembrane collagen, and the like, according to their structures. Is generally white, transparent powder, and has elongated rod shape with relative molecular mass ranging from about 2kD to 300 kD. The collagen has strong extension force, is insoluble in cold water, dilute acid and dilute alkali solution, and has good water retention and emulsibility. The collagen is mixed with other synthetic or natural polymer with different physical and chemical properties to form a multiphase solid material, and the collagen and other polymer are mutually supplemented to form a collagen-based composite material.
Ethylene thiourea is generally used for products such as wires, cables, rubbers, pipe belts, rubber shoes, rain shoes, raincoats and the like, and is also used for fine chemical crystal intermediates, antioxidants, insecticides, dye medicines and synthetic resins.
The pure 2-mercaptobenzimidazole is white or light yellow fine powder crystal, has no toxicity and bitter taste, and is soluble in ether, acetone and ethyl acetate, and has a purity of 1.40-1.44 relative to Density1.40 and Melting _ point of not lower than 285 ℃. The copper plating brightener N, SP is used in combination with copper plating brightener to brighten and level the plated layer and to increase the working current density. The epoxy resin can be used as an epoxy resin curing agent, can improve mechanical properties of products such as bending, stretching and compression, can improve electrical insulation property, can improve chemical resistance of chemical agents, and can be used as a copper antirust agent for printed circuit boards and integrated circuits.
The tetrahydrothiazolethione is mainly used as an acidic bright copper plating additive, can obtain good brightness and leveling property, and has high brightening speed.
The sodium polydithio-dipropyl sulfonate is used as an acid copper plating brightener to obtain a decorative and functional plating layer.
The polyethylene glycol series products have no toxicity, no irritation, slightly bitter taste, good water solubility and good intermiscibility with a plurality of organic matter components. They have excellent lubricity, moisture retention, dispersibility, adhesive, antistatic agent, softening agent and the like, and are useful as plasticizers, softeners, moisturizers and the like.
The polyether is also called polyglycol ether, and is one of the most sold synthetic oils. It is a linear polymer prepared by ring-opening homopolymerization or copolymerization of ethylene oxide, propylene oxide, butylene oxide and the like serving as raw materials under the action of a catalyst. The polyether has the outstanding characteristic that the viscosity and the viscosity index of the polyether are correspondingly increased along with the increase of the molecular weight of the polyether. The kinematic viscosity of the modified polyvinyl alcohol at 50 ℃ is changed within the range of 6-1000 mm 2/s. The viscosity index of the polyether is much larger than that of mineral oil, and is about 170-245.
Another object of the present invention is to provide a method for preparing an additive for producing a graded electrolytic copper foil, comprising the steps of:
(1) preparing raw materials: preparing chlorine-containing compounds, polyether compounds, collagen, sodium polydithio-dipropyl sulfonate, polyethylene glycol, 2-mercapto benzimidazole, ethylene thiourea and thiazolidinethione;
(2) solution preparation: preparing a copper sulfate solution;
(3) adding raw materials: adding a chlorine-containing compound, a polyether compound, collagen, sodium polydithiodipropyl sulfonate, polyethylene glycol, 2-mercaptobenzimidazole, ethylene thiourea and thiazolidinethione into the copper sulfate solution in a metered manner;
(4) mixing: the raw materials are added into copper sulfate solution and mixed for 1-5min under stirring to prepare the additive for producing the gradual change type electrolytic copper foil.
Preferably, the stirring time in step (4) is 5 min.
By adopting the technical scheme, the collagen can be blended with other synthetic or natural macromolecules with different physical and chemical properties to form a multiphase solid material, the collagen and other macromolecules supplement each other in performance to form a collagen-based composite material, and the collagen-based composite material is combined with the 2-mercaptobenzimidazole, so that the characteristic of improving the mechanical properties of the product such as bending, stretching, compressing and the like in the 2-mercaptobenzimidazole can be combined with the characteristic of strong extension force. Therefore, when the copper foil is added into the electrolytic copper foil, the surface hardness of the electrolytic copper foil is increased, the time for maintaining the surface hardness is prolonged, the mechanical properties of bending, stretching and compression of the copper foil can be enhanced while the surface hardness of the copper foil is not reduced, and the copper foil is prevented from wrinkling, so that the yield of downstream processes is improved, and the production cost is reduced.
In addition, the polyether compound and the thiazolidinethione are added and mixed, and the advantages of collagen are combined, so that the bending, stretching and compression mechanical properties of the product are provided, the viscosity and the surface smoothness are increased, and copper foil wrinkles are further avoided, so that the yield of downstream processes is further improved, and the production cost is further reduced.
Drawings
FIG. 1 is a microscopic view of a copper foil to which the additive of the present invention is not added;
FIG. 2 is a microscope image of the M-side of a copper foil prepared using the additive of the present invention;
FIG. 3 is a microscope image of the copper foil anode side of a two-sided photo lithium battery prepared using the additive of the present invention.
Detailed Description
The following further describes embodiments of the present invention with reference to the drawings. It should be noted that the description of the embodiments is provided to help understanding of the present invention, but the present invention is not limited thereto. In addition, the technical features related to the respective embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
In order to solve the problem that the mechanical strength of the copper foil is influenced when the surface hardness of the electrolytic copper foil is lower in the prior art; the present invention provides the following examples if the technical contradiction that the surface hardness of the copper foil is increased to be high, which in turn leads to the reduction of the elongation of the copper foil.
Example 1
An additive for producing a graded electrolytic copper foil: the material is prepared from the following raw materials in parts by weight: 30-120 g of chlorine-containing compound, 10-150 g of polyether compound, 50-600 g of collagen, 30-600 g of sodium polydithiodipropyl sulfonate, 10-200 g of polyethylene glycol, 20-500 g of 2-mercaptobenzimidazole, 10-600 g of ethylene thiourea and 10-200 g of thiazolidinethione, wherein the molecular weight of the polyether compound is 4000, and the molecular weight of the polyethylene glycol is 6000.
The above raw materials were added to one liter of copper sulfate solution.
The molecular formula of the 2-mercapto benzimidazole is C7H6N 2S; the molecular formula of the ethylene thiourea is C3H6N 2S; the molecular formula of the thiazolidinethione is C3H5NS 2.
The structural formula of the 2-mercapto benzimidazole (C7H6N2S) is as follows:
the structural formula of ethylene thiourea (C3H6N2S) is:
the structural formula of thiazolidinethione (C3H5NS2) is:
the invention also provides a preparation method of the additive for producing the gradual change type electrolytic copper foil, which comprises the following steps:
(1) preparing raw materials: preparing chlorine-containing compounds, polyether compounds, collagen, sodium polydithio-dipropyl sulfonate, polyethylene glycol, 2-mercapto benzimidazole, ethylene thiourea and thiazolidinethione;
(2) solution preparation: preparing a copper sulfate solution;
(3) adding raw materials: adding a chlorine-containing compound, a polyether compound, collagen, sodium polydithio-dipropyl sulfonate, polyethylene glycol, 2-mercapto benzimidazole, ethylene thiourea and thiazolidinethione into each liter of copper sulfate solution;
(4) mixing: and adding the raw materials into a copper sulfate solution, and mixing for 5min under stirring to obtain the additive for producing the gradient electrolytic copper foil.
Example 2
An additive for producing a graded electrolytic copper foil, which is prepared by the following raw materials in parts by weight according to the preparation method in example 1: 100 g of chlorine-containing compound, 100 g of polyether compound, 300 g of collagen, 400 g of sodium polydithiodipropyl sulfonate, 100 g of polyethylene glycol, 300 g of 2-mercaptobenzimidazole, 500 g of ethylene thiourea and 120 g of thiazolidinethione, wherein the molecular weight of the polyether compound is 16000, and the molecular weight of the polyethylene glycol is 8000.
Example 3
An additive for producing a graded electrolytic copper foil: the preparation method comprises the following steps of preparing the following raw materials in parts by weight according to the preparation method in the embodiment 1: 120 g of chlorine-containing compound, 150 g of polyether compound, 600 g of collagen, 600 g of sodium polydithiodipropyl sulfonate, 200 g of polyethylene glycol, 500 g of 2-mercaptobenzimidazole, 600 g of ethylene thiourea and 200 g of thiazolidinethione, wherein the molecular weight of the polyether compound is 20000, and the molecular weight of the polyethylene glycol is 10000.
The additives prepared in examples 1 to 3 were applied to the preparation of electrolytic copper foil according to the process of patent application No. 201710169974.6. The physical properties of the electrolytic copper foil products obtained in examples 1 to 3 are shown in Table one:
table one: physical Properties of the electrolytic copper foil products obtained in examples 1 to 3 and comparative example
FIG. 1 is an SEM image (1000 times) of the M surface of the rough side of a product without the additive of the invention,
FIG. 2 is an M-side micrograph (1000 times) of a copper foil prepared using the additive of the present invention;
FIG. 3 is a microscope image (3000 times) of the copper foil anode side of a two-sided photo lithium battery prepared using the additive of the present invention.
As can be seen from the table I and FIGS. 1 to 3, the copper foil prepared by using the additive of the present invention can obtain a product with higher tensile strength and elongation and low roughness, thereby better avoiding the wrinkle of the copper foil, further improving the yield and further reducing the production cost. The products without the addition of the additives according to the invention appear coarser than the products to which the additives according to the invention have been added.
The embodiments of the present invention have been described in detail with reference to the accompanying drawings, but the present invention is not limited to the described embodiments. It will be apparent to those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, and the scope of protection is still within the scope of the invention.
Claims (8)
1. An additive for producing a graded electrolytic copper foil, characterized in that: the material is prepared from the following raw materials in parts by weight: 30-120 parts of chlorine-containing compound, 10-150 parts of polyether compound, 50-600 parts of collagen, 30-600 parts of sodium polydithio-dipropyl sulfonate, 10-200 parts of polyethylene glycol, 20-500 parts of 2-mercapto benzimidazole, 10-600 parts of ethylene thiourea and 10-200 parts of tetrahydrothiazole thioketone, wherein the molecular weight of the polyether compound is 4000-20000, and the molecular weight of the polyethylene glycol is 6000-10000.
2. The additive for producing a graded electrolytic copper foil according to claim 1, wherein: the material is prepared from the following raw materials in parts by weight: 30-100 parts of chlorine-containing compound, 10-100 parts of polyether compound, 50-300 parts of collagen, 30-400 parts of sodium polydithio-dipropyl sulfonate, 10-100 parts of polyethylene glycol, 20-300 parts of 2-mercapto benzimidazole, 10-400 parts of ethylene thiourea and 10-80 parts of tetrahydrothiazole thioketone, wherein the molecular weight of the polyether compound is 4000-10000, and the molecular weight of the polyethylene glycol is 6000-8000.
3. The additive for producing a graded electrolytic copper foil according to claim 1, wherein: the material is prepared from the following raw materials in parts by weight: 100-120 parts of chlorine-containing compound, 100-150 parts of polyether compound, 300-600 parts of collagen, 400-600 parts of sodium polydithio-dipropyl sulfonate, 100-200 parts of polyethylene glycol, 300-500 parts of 2-mercapto benzimidazole, 400-600 parts of ethylene thiourea and 80-200 parts of tetrahydrothiazole thione, wherein the molecular weight of the polyether compound is 10000-20000, and the molecular weight of the polyethylene glycol is 8000-10000.
4. The additive for producing a graded electrolytic copper foil according to claim 1, wherein: the material is prepared from the following raw materials in parts by weight: 80-110 parts of chlorine-containing compound, 50-120 parts of polyether compound, 200-400 parts of collagen, 450 parts of sodium polydithio-dipropyl sulfonate 350-90 parts, 50-150 parts of polyethylene glycol, 400 parts of 2-mercapto benzimidazole 250-500 parts of ethylene thiourea and 50-150 parts of tetrahydrothiazole thioketone, wherein the molecular weight of the polyether compound is 8000-18000, and the molecular weight of the polyethylene glycol is 8000-10000.
5. The additive for producing a graded electrolytic copper foil according to any one of claims 1 to 4, wherein: the material is prepared from the following raw materials in parts by weight: 100 parts of chlorine-containing compound, 100 parts of polyether compound, 300 parts of collagen, 400 parts of sodium polydithio-dipropyl sulfonate, 100 parts of polyethylene glycol, 300 parts of 2-mercapto benzimidazole, 500 parts of ethylene thiourea and 120 parts of thiazolidinethione, wherein the molecular weight of the polyether compound is 16000, and the molecular weight of the polyethylene glycol is 8000.
6. The additive for producing a graded electrolytic copper foil according to any one of claims 1 to 4, wherein: the molecular formula of the 2-mercapto benzimidazole is C7H6N 2S; the molecular formula of the ethylene thiourea is C3H6N 2S; the molecular formula of the thiazolidinethione is C3H5NS 2.
7. The method for preparing an additive for producing a graded electrolytic copper foil according to any one of claims 1 to 6, wherein: the method comprises the following steps:
(1) preparing raw materials: preparing chlorine-containing compounds, polyether compounds, collagen, sodium polydithio-dipropyl sulfonate, polyethylene glycol, 2-mercapto benzimidazole, ethylene thiourea and thiazolidinethione;
(2) solution preparation: preparing a copper sulfate solution;
(3) adding raw materials: adding chlorine-containing compounds, polyether compounds, collagen, sodium polydithio-dipropyl sulfonate, polyethylene glycol, 2-mercapto benzimidazole, ethylene thiourea and thiazolidinethione into the copper sulfate solution in a metered manner;
(4) mixing: the raw materials are added into copper sulfate solution and mixed for 1-5min under stirring to prepare the additive for producing the gradual change type electrolytic copper foil.
8. The method for preparing an additive for producing a graded electrolytic copper foil according to claim 7, wherein: and (4) stirring for 5 min.
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| CN115074787B (en) * | 2022-07-13 | 2023-11-10 | 佛冈建滔实业有限公司 | Additive for copper foil production and application thereof |
| CN115505968A (en) * | 2022-09-13 | 2022-12-23 | 江苏鑫瑞崚新材料科技有限公司 | Formula and preparation method of additive for purifying low-silver low-sulfur ultra-pure copper |
| CN115787000A (en) * | 2022-12-12 | 2023-03-14 | 江苏梦得新材料科技有限公司 | High-tensile-strength additive and preparation method thereof |
| CN117051446A (en) * | 2023-08-24 | 2023-11-14 | 江西铜博科技股份有限公司 | Additive for producing electrolytic copper foil and method for producing electrolytic copper foil |
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