CN108192056A - A kind of preparation method of the castor oil modified linear phenol-aldehyde resin of copper-clad plate - Google Patents
A kind of preparation method of the castor oil modified linear phenol-aldehyde resin of copper-clad plate Download PDFInfo
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- CN108192056A CN108192056A CN201810092928.5A CN201810092928A CN108192056A CN 108192056 A CN108192056 A CN 108192056A CN 201810092928 A CN201810092928 A CN 201810092928A CN 108192056 A CN108192056 A CN 108192056A
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- preparation
- phenol
- castor oil
- copper
- clad plate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G8/00—Condensation polymers of aldehydes or ketones with phenols only
- C08G8/28—Chemically modified polycondensates
- C08G8/32—Chemically modified polycondensates by organic acids or derivatives thereof, e.g. fatty oils
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L61/00—Compositions of condensation polymers of aldehydes or ketones; Compositions of derivatives of such polymers
- C08L61/04—Condensation polymers of aldehydes or ketones with phenols only
- C08L61/06—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
- C08L61/14—Modified phenol-aldehyde condensates
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/06—Polymer mixtures characterised by other features having improved processability or containing aids for moulding methods
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- General Chemical & Material Sciences (AREA)
- Phenolic Resins Or Amino Resins (AREA)
Abstract
The invention belongs to phenolic resin production technical field more particularly to a kind of preparation methods of the castor oil modified linear phenol-aldehyde resin of copper-clad plate.The present invention uses acidic catalyst, phenolic resin is modified with castor oil, obtained is the thermoplastic resin of line style, it is few to cure the high and low molecule volatile matter of post-crosslinking density, copper-clad plate is used to prepare, copper-clad plate toughness and heat resistance can be significantly improved, can be used for pb-free solder processing procedure, extend its service life, reduce production cost.
Description
Technical field
The invention belongs to phenolic resin production technical field more particularly to a kind of castor oil modified line style phenolic aldehyde of copper-clad plate
The preparation method of resin.
Background technology
In copper-clad plate industry, common toughened resin is tung oil modified phenolic resin, but such toughened resin belongs to thermosetting
Property phenolic resin, curing post-crosslinking density is low, and the low molecular weight volatile object contained is more, and copper-clad plate heat resistance obtained is bad, nothing
Method meets requirement of the downstream PCB client to plank heat resistance.
Invention content
The present invention in view of the deficiency of the prior art, provides a kind of copper-clad plate with castor oil modified line style phenolic aldehyde tree
The preparation method of fat.
The technical solution that the present invention solves above-mentioned technical problem is as follows：A kind of copper-clad plate is with castor oil modified line style phenolic aldehyde tree
The preparation method of fat, step are as follows：
(1) phenol, castor oil, acidic catalyst are added in reaction kettle, are heated to 100-120 DEG C of heat preservation 2-3h；
(2) batch mixing of step (1) under stirring is cooled to 50-70 DEG C, adds in aldehyde material and acidic catalyst,
It is warming up to 100-110 DEG C of reaction 2-3h；
(3) after the product of step (2) being vacuumized dehydration, solvent is added in get to the castor oil modified line of yellow transparent
Type phenolic resin.
Wherein, in step (1) and step (2), the acidic catalyst is oxalic acid, acetic acid, benzoic acid, hydrochloric acid, sulfuric acid
Or one or more of nitric acid mixing.
In step (1), the dosage molar ratio of phenol and castor oil is (5-6)：1.
The dosage molar ratio of phenol and aldehyde material is 1：(0.9-1.1).
Acidic catalyst total weight is the 0.9-1.1% of phenol weight in step (1) neutralization procedure (2).
In step (1), acidic catalyst weight is the 60-70% of acidic catalyst total weight.
In step (2), the aldehyde material is mixed for one or more of formaldehyde, metaformaldehyde or paraformaldehyde
It closes.
In step (3), the solvent is the mixing of one or more of methanol, acetone, ethyl alcohol or butanone.
In step (3), the solvent dosage is 3~4 times of step (1) phenol weight.
The features of the present invention and advantageous effect are：
The present invention is modified phenolic resin with castor oil, obtained is the thermoplasticity of line style using acidic catalyst
Resin, the curing high and low molecule volatile matter of post-crosslinking density is few, is used to prepare copper-clad plate, can significantly improve copper-clad plate toughness and resistance to
It is hot, it can be used for pb-free solder processing procedure, extend its service life, reduce production cost.
Specific embodiment
The principle of the present invention and feature are described below in conjunction with example, the given examples are served only to explain the present invention, and
It is non-to be used to limit the scope of the present invention.
Embodiment 1
A kind of preparation method of the castor oil modified linear phenol-aldehyde resin of copper-clad plate, step are as follows：
(1) it is 5 according to molar ratio by phenol and castor oil:1 is added in reaction kettle, adds in the acid of phenol weight 0.54%
Property catalyst, be heated to 100 DEG C heat preservation 2h；
(2) 70 DEG C are cooled under stirring, adds in formaldehyde and acidic catalyst, is warming up to 105 DEG C of reaction 2h；Phenol
Molar ratio with formaldehyde is 1:0.9, the weight of acidic catalyst is phenol weight 0.36%；
(3) product of step (2) is vacuumized into dehydration, adds in step (1) phenol and feed intake the solvent first of 3 times of dosages of quality
Alcohol is to get to the castor oil modified linear phenol-aldehyde resin of yellow transparent.
Embodiment 2
A kind of preparation method of the castor oil modified linear phenol-aldehyde resin of copper-clad plate, step are as follows：
(1) it is 5.5 according to molar ratio by phenol and castor oil:1 is added in reaction kettle, adds in phenol weight 0.585%
Acidic catalyst, be heated to 100 DEG C heat preservation 2h；
(2) 70 DEG C are cooled under stirring, adds in formaldehyde and acidic catalyst, is warming up to 105 DEG C of reaction 2h；Phenol
Molar ratio with formaldehyde is 1:1, the weight of acidic catalyst is phenol weight 0.315%；
(3) product of step (2) is vacuumized into dehydration, adds in step (1) phenol and feed intake the solvent first of 3.5 times of dosages of quality
Alcohol is to get to the castor oil modified linear phenol-aldehyde resin of yellow transparent.
Embodiment 3
A kind of preparation method of the castor oil modified linear phenol-aldehyde resin of copper-clad plate, step are as follows：
(1) it is 6 according to molar ratio by phenol and castor oil:1 is added in reaction kettle, adds in the acid of phenol weight 0.63%
Property catalyst, be heated to 100 DEG C heat preservation 2h；
(2) 70 DEG C are cooled under stirring, adds in formaldehyde and acidic catalyst, is warming up to 105 DEG C of reaction 2h；Phenol
Molar ratio with formaldehyde is 1:1.1, the weight of acidic catalyst is phenol weight 0.27%；
(3) product of step (2) is vacuumized into dehydration, adds in step (1) phenol and feed intake the solvent first of 4 times of dosages of quality
Alcohol is to get to the castor oil modified linear phenol-aldehyde resin of yellow transparent.
Using linear phenol-aldehyde resin castor oil modified made from the present embodiment as the curing toughening of composite-based copper clad plate lining
Agent, for producing CEM-1 copper-clad plates, every leading indicator such as the following table 1.
Comparative example 1
By the use of tung oil modified phenolic resin as the curing toughener of composite-based copper clad plate lining, copper is covered for producing CEM-1
Plate, every leading indicator such as the following table 1.
Table 1
As can be seen from Table 1, copper-clad plate heat resistance produced by the present invention is significantly improved, and plank toughness is preferable, other
It has excellent performance, the market demand can be met.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all the present invention spirit and
Within principle, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention.
Claims (9)
1. a kind of copper-clad plate preparation method of castor oil modified linear phenol-aldehyde resin, which is characterized in that step is as follows：
(1) phenol, castor oil, acidic catalyst are added in reaction kettle, are heated to 100-120 DEG C of heat preservation 2-3h；
(2) batch mixing of step (1) under stirring is cooled to 50-70 DEG C, adds in aldehyde material and acidic catalyst, heating
To 100-110 DEG C of reaction 2-3h；
(3) after the product of step (2) being vacuumized dehydration, solvent is added in get to the castor oil modified line style phenol of yellow transparent
Urea formaldehyde.
2. preparation method according to claim 1, which is characterized in that in step (1) and step (2), the acidity is urged
Agent is the mixing of one or more of oxalic acid, acetic acid, benzoic acid, hydrochloric acid, sulfuric acid or nitric acid.
3. preparation method according to claim 1, which is characterized in that in step (1), the dosage mole of phenol and castor oil
Than for (5-6)：1.
4. preparation method according to claim 1, which is characterized in that the dosage molar ratio of phenol and aldehyde material is 1：
(0.9-1.1)。
5. preparation method according to claim 1, which is characterized in that acidic catalyst is total in step (1) neutralization procedure (2)
Weight is the 0.9-1.1% of phenol weight.
6. preparation method according to claim 5, which is characterized in that in step (1), acidic catalyst weight is urged for acidity
The 60-70% of agent total weight.
7. preparation method according to claim 1, which is characterized in that in step (2), the aldehyde material for formaldehyde,
The mixing of one or more of metaformaldehyde or paraformaldehyde.
8. preparation method according to claim 1, which is characterized in that in step (3), the solvent for methanol, acetone,
The mixing of one or more of ethyl alcohol or butanone.
9. preparation method according to claim 1, which is characterized in that in step (3), the solvent dosage is step
(1) 3~4 times of phenol weight.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810092928.5A CN108192056A (en) | 2018-01-31 | 2018-01-31 | A kind of preparation method of the castor oil modified linear phenol-aldehyde resin of copper-clad plate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810092928.5A CN108192056A (en) | 2018-01-31 | 2018-01-31 | A kind of preparation method of the castor oil modified linear phenol-aldehyde resin of copper-clad plate |
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| Publication Number | Publication Date |
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| CN108192056A true CN108192056A (en) | 2018-06-22 |
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| CN201810092928.5A Pending CN108192056A (en) | 2018-01-31 | 2018-01-31 | A kind of preparation method of the castor oil modified linear phenol-aldehyde resin of copper-clad plate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115417959A (en) * | 2022-09-30 | 2022-12-02 | 北京彤程创展科技有限公司 | Biomass fatty acid modified resin, preparation method thereof, rubber composition and product |
| CN117326886A (en) * | 2022-06-24 | 2024-01-02 | 比亚迪股份有限公司 | Slurry for ceramic copper-clad part, and preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DD266574A1 (en) * | 1987-12-18 | 1989-04-05 | Sprela Werke Spremberg Veb | METHOD FOR THE PRODUCTION OF MODIFIED NOVOLAK TYPE PF RESINS |
| CN1072188A (en) * | 1991-11-05 | 1993-05-19 | 成都科技大学 | The manufacturing of tung oil modified linear phenol-aldehyde resin and application |
| CN1803874A (en) * | 2005-11-25 | 2006-07-19 | 华南理工大学 | Epoxy plant oil modified phenol-formaldehyde resin, its preparation method and application |
| CN107097508A (en) * | 2017-05-10 | 2017-08-29 | 山东金宝科创股份有限公司 | A kind of high heat-resisting, highly heat-conductive copper-clad plate preparation method |
-
2018
- 2018-01-31 CN CN201810092928.5A patent/CN108192056A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DD266574A1 (en) * | 1987-12-18 | 1989-04-05 | Sprela Werke Spremberg Veb | METHOD FOR THE PRODUCTION OF MODIFIED NOVOLAK TYPE PF RESINS |
| CN1072188A (en) * | 1991-11-05 | 1993-05-19 | 成都科技大学 | The manufacturing of tung oil modified linear phenol-aldehyde resin and application |
| CN1803874A (en) * | 2005-11-25 | 2006-07-19 | 华南理工大学 | Epoxy plant oil modified phenol-formaldehyde resin, its preparation method and application |
| CN107097508A (en) * | 2017-05-10 | 2017-08-29 | 山东金宝科创股份有限公司 | A kind of high heat-resisting, highly heat-conductive copper-clad plate preparation method |
Non-Patent Citations (2)
| Title |
|---|
| 王幸之 等: "《单片机应用系统电磁干扰与抗干扰技术》", 28 February 2006, 北京航空航天大学出版社 * |
| 金鸿 等: "《印制电路技术》", 31 December 2003, 化学工业出版社 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117326886A (en) * | 2022-06-24 | 2024-01-02 | 比亚迪股份有限公司 | Slurry for ceramic copper-clad part, and preparation method and application thereof |
| CN115417959A (en) * | 2022-09-30 | 2022-12-02 | 北京彤程创展科技有限公司 | Biomass fatty acid modified resin, preparation method thereof, rubber composition and product |
| CN115417959B (en) * | 2022-09-30 | 2024-05-24 | 北京彤程创展科技有限公司 | Biomass fatty acid modified resin, preparation method thereof, rubber composition and product |
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