CN110684315A - Preparation process of high-uniformity phenolic resin - Google Patents
Preparation process of high-uniformity phenolic resin Download PDFInfo
- Publication number
- CN110684315A CN110684315A CN201910916224.XA CN201910916224A CN110684315A CN 110684315 A CN110684315 A CN 110684315A CN 201910916224 A CN201910916224 A CN 201910916224A CN 110684315 A CN110684315 A CN 110684315A
- Authority
- CN
- China
- Prior art keywords
- phenolic resin
- uniformity
- titanate
- stirring
- mixed solution
- 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.)
- Pending
Links
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 239000005011 phenolic resin Substances 0.000 title claims abstract description 48
- 229920001568 phenolic resin Polymers 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 30
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 24
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000011259 mixed solution Substances 0.000 claims abstract description 18
- 239000000243 solution Substances 0.000 claims abstract description 13
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000004519 manufacturing process Methods 0.000 claims abstract description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 8
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 4
- 229910021529 ammonia Inorganic materials 0.000 claims description 4
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 4
- 229910052750 molybdenum Inorganic materials 0.000 claims description 4
- 239000011733 molybdenum Substances 0.000 claims description 4
- JMXKSZRRTHPKDL-UHFFFAOYSA-N titanium ethoxide Chemical compound [Ti+4].CC[O-].CC[O-].CC[O-].CC[O-] JMXKSZRRTHPKDL-UHFFFAOYSA-N 0.000 claims description 4
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims description 4
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 4
- 229910052721 tungsten Inorganic materials 0.000 claims description 4
- 239000010937 tungsten Substances 0.000 claims description 4
- 238000000034 method Methods 0.000 abstract description 3
- 239000006185 dispersion Substances 0.000 abstract description 2
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 238000003860 storage Methods 0.000 abstract description 2
- 239000002245 particle Substances 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001879 gelation Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The invention relates to a preparation process of high-uniformity phenolic resin, which comprises the following steps: 1) adding titanate into acetylacetone under stirring at the temperature of 20-24 ℃, and continuously stirring until a uniform mixed solution A is formed; 2) slowly dropwise adding the mixed solution A into a phenolic resin ethanol solution with the gel content of 66-68 wt% under stirring at the temperature of 20-24 ℃, wherein the weight ratio of the phenolic resin ethanol solution to acetylacetone to titanate is 100: 15-30: 2-4, the dropwise adding speed of the mixed solution A is 4-6 ml/min, and the stirring speed is 100-300 r/min; 3) stirring for 0.5-0.8 h at 20-25 ℃ to obtain the high-uniformity phenolic resin. The invention has the advantages that: the preparation method has the advantages of simple process, low production cost, low energy consumption, safety, environmental protection, low requirement on equipment performance, easy industrial stable production, uniform prepared phenolic resin dispersion system, good stability and suitability for storage.
Description
Technical Field
The invention relates to a preparation process of high-uniformity phenolic resin.
Background
The heat resistance of the common phenolic resin is not ideal enough, the thermal decomposition phenomenon is serious when the temperature is over 300 ℃, and the carbon residue rate is only about 40% when the temperature is over 800 ℃. In order to improve the heat resistance of the phenolic resin, the phenolic resin needs to be modified.
Method for modifying phenolic resin by inorganic nano particles in prior art and obtained nano TO2The particles are easily agglomerated and unevenly dispersed in the reaction system. Resulting in insufficient homogeneity of the resulting phenolic resin. The prior art also uses titanate to modify boron phenolic resin, but titanate reacts rapidly with water to produce TiO2Precipitation, little addition amount, difficult control of reaction, easy gelation and difficult formation of uniform phenolic resin.
Disclosure of Invention
The invention provides a preparation process of high-uniformity phenolic resin, aiming at overcoming the defects in the prior art and realizing the production of the high-uniformity phenolic resin.
The technical solution of the invention is as follows: a preparation process of high-uniformity phenolic resin comprises the following steps:
1) adding titanate into acetylacetone under stirring at the temperature of 20-24 ℃, and continuously stirring until a uniform mixed solution A is formed;
2) slowly dropwise adding the mixed solution A into a phenolic resin ethanol solution with the gel content of 66-68 wt% under stirring at the temperature of 20-24 ℃, wherein the weight ratio of the phenolic resin ethanol solution to acetylacetone to titanate is 100: 15-30: 2-4, the dropwise adding speed of the mixed solution A is 4-6 ml/min, and the stirring speed is 100-300 r/min;
3) stirring for 0.5-0.8 h at 20-25 ℃ to obtain the high-uniformity phenolic resin.
Preferably, the titanate is one or more of ethyl titanate, isopropyl titanate and butyl titanate.
Preferably, the phenolic resin is one or more of ammonia phenolic resin, molybdenum phenolic resin and tungsten phenolic resin.
The invention has the advantages that: the preparation method has the advantages of simple process, low production cost, low energy consumption, safety, environmental protection, low requirement on equipment performance, easy industrial stable production, uniform prepared phenolic resin dispersion system, good stability and suitability for storage.
Detailed Description
The present invention will be described in further detail with reference to examples and specific embodiments.
Example 1
A preparation process of high-uniformity phenolic resin comprises the following steps:
1) adding butyl titanate into acetylacetone under stirring at 20 ℃, and continuously stirring until a uniform mixed solution A is formed;
2) slowly dropwise adding the mixed solution A into a molybdenum phenolic resin ethanol solution with the gel content of 66 wt% under stirring at the temperature of 20 ℃, wherein the weight ratio of the molybdenum phenolic resin ethanol solution to acetylacetone to butyl titanate is 100:15:4, the dropwise adding speed of the mixed solution A is 4ml/min, and the stirring speed is 100 r/min;
3) stirring for 0.5h at 20 ℃ to obtain the high-uniformity phenolic resin.
The product is clear and transparent after being stored for 12 months at 20 ℃, and no floccule or small crystal particles can be seen by naked eyes.
Example 2
A preparation process of high-uniformity phenolic resin comprises the following steps:
1) adding isopropyl titanate into acetylacetone under stirring at 24 ℃, and continuing stirring until a uniform mixed solution A is formed;
2) slowly dropwise adding the mixed solution A into a tungsten phenolic resin ethanol solution with gel content of 68 wt% under stirring at the temperature of 24 ℃, wherein the weight ratio of the tungsten phenolic resin ethanol solution to the acetylacetone to the isopropyl titanate is 100:30:2, the dropwise adding speed of the mixed solution A is 6ml/min, and the stirring speed is 300 r/min;
3) stirring for 0.8h at 25 ℃ to obtain the high-uniformity phenolic resin.
The product is clear and transparent after being stored for 12 months at 20 ℃, and no floccule or small crystal particles can be seen by naked eyes.
Example 3
A preparation process of high-uniformity phenolic resin comprises the following steps:
1) adding ethyl titanate into acetylacetone under stirring at 22 ℃, and continuing stirring until a uniform mixed solution A is formed;
2) slowly dripping the mixed solution A into an ammonia phenolic resin ethanol solution with the gel content of 67 wt% under stirring at the temperature of 22 ℃, wherein the weight ratio of the ammonia phenolic resin ethanol solution to the acetylacetone to the ethyl titanate is 100:20:3, the dripping speed of the mixed solution A is 5ml/min, and the stirring speed is 200 r/min;
3) stirring for 0.6h at 22 ℃ to obtain the high-uniformity phenolic resin.
The product is clear and transparent after being stored for 12 months at 20 ℃, and no floccule or small crystal particles can be seen by naked eyes.
All the above components are prior art, and those skilled in the art can use any model and existing design that can implement their corresponding functions.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various changes and modifications can be made without departing from the inventive concept of the present invention, and these changes and modifications are all within the scope of the present invention.
Claims (3)
1. A preparation process of high-uniformity phenolic resin is characterized by comprising the following steps:
1) adding titanate into acetylacetone under stirring at the temperature of 20-24 ℃, and continuously stirring until a uniform mixed solution A is formed;
2) slowly dropwise adding the mixed solution A into a phenolic resin ethanol solution with the gel content of 66-68 wt% under stirring at the temperature of 20-24 ℃, wherein the weight ratio of the phenolic resin ethanol solution to acetylacetone to titanate is 100: 15-30: 2-4, the dropwise adding speed of the mixed solution A is 4-6 ml/min, and the stirring speed is 100-300 r/min;
3) stirring for 0.5-0.8 h at 20-25 ℃ to obtain the high-uniformity phenolic resin.
2. The process for preparing high-uniformity phenolic resin according to claim 1, wherein the titanate is one or more of ethyl titanate, isopropyl titanate and butyl titanate.
3. A process for preparing high-uniformity phenolic resin according to claim 1 or 2, wherein said phenolic resin is one or more of ammonia phenolic resin, molybdenum phenolic resin and tungsten phenolic resin.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910916224.XA CN110684315A (en) | 2019-09-26 | 2019-09-26 | Preparation process of high-uniformity phenolic resin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910916224.XA CN110684315A (en) | 2019-09-26 | 2019-09-26 | Preparation process of high-uniformity phenolic resin |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110684315A true CN110684315A (en) | 2020-01-14 |
Family
ID=69110189
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910916224.XA Pending CN110684315A (en) | 2019-09-26 | 2019-09-26 | Preparation process of high-uniformity phenolic resin |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110684315A (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106117964A (en) * | 2016-06-24 | 2016-11-16 | 北京玻钢院复合材料有限公司 | A kind of modified boron containing phenolic resin and preparation method and application |
| CN109160988A (en) * | 2018-10-11 | 2019-01-08 | 北京玻钢院复合材料有限公司 | The preparation method of titanium-modified phenolic resin |
-
2019
- 2019-09-26 CN CN201910916224.XA patent/CN110684315A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106117964A (en) * | 2016-06-24 | 2016-11-16 | 北京玻钢院复合材料有限公司 | A kind of modified boron containing phenolic resin and preparation method and application |
| CN109265912A (en) * | 2016-06-24 | 2019-01-25 | 北京玻钢院复合材料有限公司 | A kind of titanium modified boron containing phenolic resin and the preparation method and application thereof |
| CN109160988A (en) * | 2018-10-11 | 2019-01-08 | 北京玻钢院复合材料有限公司 | The preparation method of titanium-modified phenolic resin |
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| PB01 | Publication | ||
| PB01 | Publication | ||
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| SE01 | Entry into force of request for substantive examination | ||
| CB02 | Change of applicant information |
Address after: 214426 No.8 Xinhua Road, Xinqiao Town, Jiangyin City, Wuxi City, Jiangsu Province Applicant after: Jiangyin Bailida industrial cloth Co.,Ltd. Address before: 214426 No.8 Xinhua Road, Xinqiao Town, Jiangyin City, Wuxi City, Jiangsu Province Applicant before: JIANGSU BAILIDA Co.,Ltd. |
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| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20200114 |
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| RJ01 | Rejection of invention patent application after publication |