CN112133469B - Mixed organic solvent for preparing high-temperature sintering conductive slurry - Google Patents
Mixed organic solvent for preparing high-temperature sintering conductive slurry Download PDFInfo
- Publication number
- CN112133469B CN112133469B CN202011047093.5A CN202011047093A CN112133469B CN 112133469 B CN112133469 B CN 112133469B CN 202011047093 A CN202011047093 A CN 202011047093A CN 112133469 B CN112133469 B CN 112133469B
- Authority
- CN
- China
- Prior art keywords
- monophenyl ether
- glycol monophenyl
- weight percent
- organic solvent
- fatty acid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
Landscapes
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Conductive Materials (AREA)
Abstract
The invention relates to a mixed organic solvent for preparing high-temperature sintering conductive slurry, belonging to the technical field of oily organic solvents. Comprises 10 to 60 weight percent of fatty acid ester with a phenylate structure, 10 to 60 weight percent of butyl carbitol acetate, 0.1 to 10 weight percent of at least one of 2,2, 4-trimethyl-1, 3-pentanediol monoisobutyrate and 2,2, 4-trimethyl-1, 3-pentanediol diisobutyrate, 10 to 30 weight percent of dimethyl adipate, 0.1 to 0.5 weight percent of gamma-methacryloxypropyl trimethoxysilane and 0.5 to 1.5 weight percent of silicone oil. The preparation method has the advantages that the preparation method has the characteristics of good resin solubility, good metal particle wettability, no volatilization at room temperature, stable volatilization at high temperature and the like, can well dissolve various resins commonly used by the photovoltaic front silver paste, and is proved by experiments to be more suitable for the requirements of silver paste printing and sintering compared with the traditional single solvent system; the method has the advantages of simple reaction conditions and high product yield, and has good application prospects in the photovoltaic industry and the related fields of electronic conductive paste.
Description
Technical Field
The invention belongs to the technical field of oily organic solvents, and particularly relates to a mixed organic solvent for preparing high-temperature sintering conductive slurry.
Background
The oily organic solvent has wide application, the most common aliphatic hydrocarbon solvents are mostly used for coatings and printing ink, and the long-carbon-chain alcohol ester solvents are mostly used in the directions of cosmetics, spices, medicines, electronic paste and the like. Solvents also play an important role in the metal conductive pastes used in the photovoltaic industry.
The metal conductive paste is one of the most important materials in the field of the electronic industry. With the continuous development of the industry, the requirements on the performances of slurry conductivity, printing, welding and the like are continuously improved. The front-side silver paste for the photovoltaic solar cell needs to be subjected to steps of printing, drying, sintering and the like in the using process, and the quality of the final solar cell can be ensured only by meeting the special requirements of each step on the paste.
The high-temperature sintering conductive paste requires that the used solvent has the characteristics of slow volatilization under room-temperature printing conditions, stable volatilization in the drying stage, moderate solvent property for organic resin and the like, which is usually difficult to meet by a single solvent. Therefore, most manufacturers of high-temperature sintering conductive paste will also use mixed solvent as the solvent of the conductive paste.
Disclosure of Invention
The invention provides a mixed organic solvent for preparing high-temperature sintering conductive paste, which is suitable for the solvent proportion of the front silver paste of a solar cell.
The technical scheme adopted by the invention is that the traditional Chinese medicine is prepared from the following raw materials:
10-60 wt% of fatty acid ester containing phenylate structure;
10-60 wt% of butyl carbitol acetate;
0.1-10 wt% of at least one of 2,2, 4-trimethyl-1, 3-pentanediol monoisobutyrate and 2,2, 4-trimethyl-1, 3-pentanediol diisobutyrate;
10-30 wt% of dimethyl adipate;
0.1-0.5 wt% of gamma-methacryloxypropyltrimethoxysilane;
0.5-1.5 wt% of silicone oil.
The fatty acid ester containing the phenylether structure is prepared by the following raw materials and methods:
the molar ratio of the alcohol containing the phenylether structure to the fatty acid anhydride or the succinic anhydride is 1 (1.1-1.5), 10-20 wt% of toluene and a proper amount of sulfonic acid-based molecular sieve;
adding a water separator and a spherical condenser pipe on a round-bottom flask, heating the flask in an oil bath under the condition of magnetic stirring until toluene refluxes, and keeping the toluene to stably reflux for 2 to 8 hours; taking down the water separator and installing a dryer; and (5) cooling the mixed solution to room temperature, carrying out reduced pressure distillation on the mixed solution, and collecting the main fraction.
The alcohol containing the phenylate structure comprises ethylene glycol monophenyl ether, ethylene glycol mono-p-toluyl ether, propylene glycol monophenyl ether, butanediol monophenyl ether or triethylene glycol monophenyl ether.
The fatty acid anhydride of the present invention includes acetic anhydride, propionic anhydride or butyric anhydride.
The succinic anhydride of the present invention includes dodecenyl succinic anhydride, tetradecenyl succinic anhydride, hexadecenyl succinic anhydride or octadecenyl succinic anhydride.
The fatty acid ester containing the phenylether structure comprises one or more of ethylene glycol monophenyl ether acetate, ethylene glycol monophenyl ether butyrate, diethylene glycol monophenyl ether acetate, diethylene glycol monophenyl ether butyrate, ethylene glycol monoparatoluyl ether acetate, ethylene glycol monoparatoluyl ether butyrate, diethylene glycol monoparatoluyl ether acetate, diethylene glycol monoparatoluyl ether butyrate, propylene glycol monophenyl ether acetate, propylene glycol monophenyl ether butyrate, dipropylene glycol monophenyl ether acetate or dipropylene glycol monophenyl ether butyrate.
The invention has the advantages that the solvent takes fatty acid ester with a phenyl ether structure, butyl carbitol acetate, 2, 4-trimethyl-1, 3-pentanediol monoisobutyrate, 2, 4-trimethyl-1, 3-pentanediol diisobutyrate and dimethyl adipate as basic solvents, has different boiling points and polarities, and can be mixed to prepare a mixed solvent suitable for printing and sintering high-temperature sintering conductive paste; the gamma-methacryloxypropyltrimethoxysilane can improve the affinity of the conductive particles and organic matters; the silicone oil can provide good printing performance and is more suitable for the solvent proportion of the front silver paste of the solar cell. In the preparation of fatty acid ester containing a phenylether structure, the esterification reaction condition can also adopt the conventional alkaline esterification reaction condition, but the yield is much lower than the acid catalysis esterification reaction condition; the reaction device, the toluene reflux operation and the addition of the sulfonic acid-based molecular sieve are all used for promoting the forward progress of the reaction, and the yield of the reaction can be changed by enhancing or weakening the auxiliary conditions; the acid anhydride can be replaced by the corresponding acid of the acid anhydride, and the toluene reflux time is increased so as not to lose the yield; the invention has the characteristics of good solubility to resin, good wettability to metal particles, no volatilization at room temperature, stable volatilization at high temperature and the like, can well dissolve various resins commonly used by the photovoltaic front silver paste, and is proved by experiments to be more suitable for the requirements of silver paste printing and sintering compared with the traditional single solvent system; the method has the advantages of simple reaction conditions and high product yield, and has good application prospects in the photovoltaic industry and the related fields of electronic conductive paste.
Drawings
FIG. 1 is a drawing of a toluene reflux experimental apparatus.
Detailed Description
Example 1
Is prepared from the following raw materials:
ethylene glycol monophenyl ether acetate 60 wt%;
10 wt% of butyl carbitol acetate;
2,2, 4-trimethyl-1, 3-pentanediol monoisobutyrate 5.4 wt%;
24 wt% of dimethyl adipate;
0.1 wt% of gamma-methacryloxypropyltrimethoxysilane;
1.0 wt% of silicone oil;
the ethylene glycol monophenyl ether acetate is prepared by the following raw materials and methods:
the molar ratio of ethylene glycol monophenyl ether to acetic anhydride is 1:1.5, toluene is 20 wt%, and a proper amount of sulfonic acid-based molecular sieve;
a water separator 2 and a spherical condenser 3 are additionally arranged on a round-bottom flask 1, the mixture is heated in an oil bath under the condition of magnetic stirring until toluene refluxes, and the toluene is kept to stably reflux for 8 hours; taking down the water separator and installing a dryer; and (5) cooling the mixed solution to room temperature, carrying out reduced pressure distillation on the mixed solution, and collecting the main fraction.
Example 2
Is prepared from the following raw materials:
10 wt% of propylene glycol monophenyl ether acetate;
60 wt% of butyl carbitol acetate;
1 wt% of 2,2, 4-trimethyl-1, 3-pentanediol diisobutyrate;
28 wt% of dimethyl adipate;
0.5 wt% of gamma-methacryloxypropyltrimethoxysilane;
0.5 wt% of silicone oil.
The propylene glycol monophenyl ether acetate is prepared by the following raw materials and methods:
the mol ratio of the propylene glycol monophenyl ether to the acetic anhydride is 1:1.1, the toluene accounts for 15 wt%, and a proper amount of sulfonic acid-based molecular sieve;
a water separator 2 and a spherical condenser 3 are additionally arranged on a round-bottom flask 1, the mixture is heated in an oil bath under the condition of magnetic stirring until toluene refluxes, and the toluene is kept to stably reflux for 4 hours; taking down the water separator and installing a dryer; and (5) cooling the mixed solution to room temperature, carrying out reduced pressure distillation on the mixed solution, and collecting the main fraction.
Example 3
Is prepared from the following raw materials:
propylene glycol monophenyl ether butyrate 35 wt%;
35 wt% of butyl carbitol acetate;
5 wt% of 2,2, 4-trimethyl-1, 3-pentanediol monoisobutyrate, 5 wt% of 2,2, 4-trimethyl-1, 3-pentanediol diisobutyrate;
18.2 wt% dimethyl adipate;
0.3 wt% of gamma-methacryloxypropyltrimethoxysilane;
1.5 wt% of silicone oil.
The propylene glycol monophenyl ether butyrate is prepared from the following raw materials by the method:
the mol ratio of the propylene glycol monophenyl ether to the butyric anhydride is 1:1.3, the toluene accounts for 10 wt%, and a proper amount of sulfonic acid-based molecular sieve;
a water separator 2 and a spherical condenser 3 are additionally arranged on a round-bottom flask 1, the mixture is heated in an oil bath under the condition of magnetic stirring until toluene refluxes, and the toluene is kept to stably reflux for 2 hours; taking down the water separator and installing a dryer; and (5) cooling the mixed solution to room temperature, carrying out reduced pressure distillation on the mixed solution, and collecting the main fraction.
Claims (4)
1. The mixed organic solvent for preparing the high-temperature sintering conductive paste is characterized by being prepared from the following raw materials:
10-60 wt% of fatty acid ester containing phenylate structure;
10-60 wt% of butyl carbitol acetate;
0.1-10 wt% of at least one of 2,2, 4-trimethyl-1, 3-pentanediol monoisobutyrate and 2,2, 4-trimethyl-1, 3-pentanediol diisobutyrate;
10-30 wt% of dimethyl adipate;
0.1-0.5 wt% of gamma-methacryloxypropyltrimethoxysilane;
0.5-1.5 wt% of silicone oil;
wherein: the fatty acid ester containing the phenylether structure is prepared by the following raw materials and methods:
the molar ratio of the alcohol containing the phenylether structure to the fatty acid anhydride is 1 (1.1-1.5), 10-20 wt% of toluene and a proper amount of sulfonic acid-based molecular sieve;
adding a water separator and a spherical condenser pipe on a round-bottom flask, heating the flask in an oil bath under the condition of magnetic stirring until toluene refluxes, and keeping the toluene to stably reflux for 2 to 8 hours; taking down the water separator and installing a dryer; and (5) cooling the mixed solution to room temperature, carrying out reduced pressure distillation on the mixed solution, and collecting the main fraction.
2. The mixed organic solvent for preparing the high-temperature sintering conductive paste according to claim 1, wherein: the alcohol containing a phenylate structure comprises ethylene glycol monophenyl ether, ethylene glycol mono-p-toluyl ether, propylene glycol monophenyl ether, butanediol monophenyl ether or triethylene glycol monophenyl ether.
3. The mixed organic solvent for preparing the high-temperature sintering conductive paste according to claim 1, wherein: the fatty acid anhydride comprises acetic anhydride, propionic anhydride or butyric anhydride.
4. The mixed organic solvent for preparing the high-temperature sintering conductive paste according to claim 1, wherein: the fatty acid ester containing the phenyl ether structure comprises one or more of ethylene glycol monophenyl ether acetate, ethylene glycol monophenyl ether butyrate, diethylene glycol monophenyl ether acetate, diethylene glycol monophenyl ether butyrate, ethylene glycol monoparatoluyl ether acetate, ethylene glycol monoparatoluyl ether butyrate, diethylene glycol monoparatoluyl ether acetate, diethylene glycol monoparatoluyl ether butyrate, propylene glycol monophenyl ether acetate, propylene glycol monophenyl ether butyrate, dipropylene glycol monophenyl ether acetate or dipropylene glycol monophenyl ether butyrate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011047093.5A CN112133469B (en) | 2020-09-28 | 2020-09-28 | Mixed organic solvent for preparing high-temperature sintering conductive slurry |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011047093.5A CN112133469B (en) | 2020-09-28 | 2020-09-28 | Mixed organic solvent for preparing high-temperature sintering conductive slurry |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN112133469A CN112133469A (en) | 2020-12-25 |
| CN112133469B true CN112133469B (en) | 2022-03-11 |
Family
ID=73844525
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011047093.5A Active CN112133469B (en) | 2020-09-28 | 2020-09-28 | Mixed organic solvent for preparing high-temperature sintering conductive slurry |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112133469B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115215745A (en) * | 2022-09-07 | 2022-10-21 | 成都中金黎阳新材料科技有限公司 | Synthesis of diethylene glycol phenyl ether acetate and application of diethylene glycol phenyl ether acetate in high-temperature and low-temperature slurry |
| CN116013577B (en) * | 2023-02-21 | 2023-06-23 | 长春黄金研究院有限公司 | Preparation method of high-temperature sintering conductive paste |
Family Cites Families (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1236470C (en) * | 2003-07-07 | 2006-01-11 | 西安交通大学 | Fluorescent powder paste composition for plasma display device and method of preparing fluorescent powder film |
| US8324294B2 (en) * | 2011-03-07 | 2012-12-04 | Xerox Corporation | Solvent-based inks comprising silver nanoparticles |
| CN102903420B (en) * | 2011-07-28 | 2016-02-03 | 比亚迪股份有限公司 | A kind of electrocondution slurry and preparation method thereof |
| CN102659586A (en) * | 2012-04-18 | 2012-09-12 | 耒阳优威新材料有限责任公司 | Method for preparing 1,6-hexanediol diacrylate |
| WO2015087811A1 (en) * | 2013-12-09 | 2015-06-18 | 株式会社ダイセル | Solvent composition for electric device production |
| CN104164283B (en) * | 2014-08-19 | 2019-09-17 | 清华大学 | Micro emulsion metalworking fluid |
| CN104262233B (en) * | 2014-08-20 | 2017-01-25 | 四川大学 | Phthalimide-containing phthalonitrile monomer and its preparation method and use |
| WO2017121740A1 (en) * | 2016-01-15 | 2017-07-20 | Basf Se | Conductive paste |
| CN110600162B (en) * | 2019-10-23 | 2021-04-02 | 河南农业大学 | Solar cell conductive paste and preparation method thereof |
-
2020
- 2020-09-28 CN CN202011047093.5A patent/CN112133469B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN112133469A (en) | 2020-12-25 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN112133469B (en) | Mixed organic solvent for preparing high-temperature sintering conductive slurry | |
| CN103435854B (en) | Crystalline silicon solar battery electrode slurry organic carrier and preparation method thereof | |
| CN109722932B (en) | Method for extracting cellulose from agricultural straw waste | |
| CN109801735A (en) | A kind of hetero-junction solar cell low temperature silver paste and preparation method | |
| CN103044668B (en) | Matt alkyd resin and preparation method thereof | |
| CN105081348A (en) | Method for preparing particle-free and high-purity silver nanowires under atmospheric pressure with one-pot method | |
| CN113571228A (en) | Front conductive silver paste for crystalline silicon solar cell and preparation method thereof | |
| CN104844542A (en) | Method for preparing gamma-valerolactone by levulinic acid ester without solvents | |
| CN103193833A (en) | Method for preparing monosaccharide ester and polyphenol product from biomasses by pressurizing, liquefying and directionally extracting and separating | |
| CN105949439B (en) | A kind of preparation method of watersoluble modified epoxy resin | |
| CN107903224A (en) | Acidic catalyst and hydrogenation catalyst concerted catalysis carbohydrate one kettle way prepare γ valerolactones | |
| CN108940258B (en) | Weak acid catalyst for synthesizing 2,2, 4-trimethylpentanediol diisobutyrate | |
| CN116013577B (en) | Preparation method of high-temperature sintering conductive paste | |
| CN116332737B (en) | Recycling method of methyl tertiary butyl ether waste solvent | |
| CN113999269B (en) | Method for promoting extraction of lignin in straws and catalytic preparation of levulinic acid and ethyl ester thereof by using ammonium-based Bronsted acidic ionic liquid | |
| CN111744553B (en) | Zirconium dodecylbenzene sulfonate catalyst and application thereof in furfuryl alcohol alcoholysis reaction | |
| CN107325890A (en) | A kind of epoxy plasticizer synthetic method based on perrhenate ions liquid | |
| CN113880790A (en) | Phase transfer catalytic synthesis method of 3, 4-epoxy cyclohexyl methyl-3 ',4' -epoxy cyclohexyl formic ether | |
| CN110201724B (en) | Hollow microsphere supported heteropolyacid catalyst and application thereof in preparation of high-viscosity cellulose acetate propionate | |
| CN107286004A (en) | The refined method of polyoxymethylene dimethyl ether | |
| CN103586052B (en) | A kind of catalyst of high acid value Fructus Zanthoxyli oil esterification acid reduction reaction and application thereof | |
| CN115449053A (en) | Lignin epoxy resin prepared by chemical reaction and toughening modification method | |
| CN115440412B (en) | Cardanol derivative-based conductive paste | |
| CN115028574B (en) | Ionic liquid and preparation method and application thereof | |
| CN113963840B (en) | Low-temperature conductive paste composition and preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |