CN101497550A - Method for producing electronic grade adamantane products - Google Patents
Method for producing electronic grade adamantane products Download PDFInfo
- Publication number
- CN101497550A CN101497550A CNA2009100584346A CN200910058434A CN101497550A CN 101497550 A CN101497550 A CN 101497550A CN A2009100584346 A CNA2009100584346 A CN A2009100584346A CN 200910058434 A CN200910058434 A CN 200910058434A CN 101497550 A CN101497550 A CN 101497550A
- Authority
- CN
- China
- Prior art keywords
- adamantane
- electronic grade
- tetrahydro
- products
- dicyclopentadiene
- 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
- ORILYTVJVMAKLC-UHFFFAOYSA-N adamantane Chemical compound C1C(C2)CC3CC1CC2C3 ORILYTVJVMAKLC-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 10
- LPSXSORODABQKT-UHFFFAOYSA-N tetrahydrodicyclopentadiene Chemical compound C1C2CCC1C1C2CCC1 LPSXSORODABQKT-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 13
- 239000003054 catalyst Substances 0.000 claims abstract description 11
- 239000002131 composite material Substances 0.000 claims abstract description 6
- 239000002904 solvent Substances 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 150000005826 halohydrocarbons Chemical class 0.000 claims description 3
- 238000006317 isomerization reaction Methods 0.000 abstract description 3
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- 150000008282 halocarbons Chemical class 0.000 abstract 1
- 150000001455 metallic ions Chemical class 0.000 abstract 1
- 239000000463 material Substances 0.000 description 9
- 229910021645 metal ion Inorganic materials 0.000 description 7
- 238000010586 diagram Methods 0.000 description 2
- ZICQBHNGXDOVJF-UHFFFAOYSA-N diamantane Chemical compound C1C2C3CC(C4)CC2C2C4C3CC1C2 ZICQBHNGXDOVJF-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- WSLDOOZREJYCGB-UHFFFAOYSA-N 1,2-Dichloroethane Chemical compound ClCCCl WSLDOOZREJYCGB-UHFFFAOYSA-N 0.000 description 1
- 235000010724 Wisteria floribunda Nutrition 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
Images
Abstract
The invention provides a method for producing an electronic-grade adamantane product, which is realized by catalytic isomerization of tetrahydrodicyclopentadiene. The method uses a homemade composite catalyst as a main catalyst with dosage of 5 to 50 percent of the tetrahydrodicyclopentadiene by weight to react at a temperature of between 30 and 180 DEG C at normal pressure. The method is characterized in that halogenated hydrocarbon is used as a solvent with dosage of 5 to 50 percent of the tetrahydrodicyclopentadiene by weight. Purity of the adamantane obtained by the method is more than or equal to 99.9 percent, and the amount of residue of metallic ions is less than or equal to 20ppm.
Description
One, technical field
The present invention relates to the production of electronic grade adamantane products, provide a kind of especially and be combined in the electronic grade adamantane products process, by using a kind of method of making composite catalyst production high purity electronic grade adamantane products by oneself at the tetrahydro-dicyclopentadiene catalytic isomerization.
Two, background technology
As everyone knows, the height of the metal ion content in the semiconductor material among the chip CPU determines the quality of this material, and metal ion content is low more, and its quality is good more.Metal ion content≤the 20ppm of this project product is the minimum diamantane material of metal ion content under the present large-scale industrial working condition, thereby is very good semiconductor material material.Just because of the metal ion content of this product is low, diamantane purity height, thereby its still present very superior sensitive materials (writing vacuum material).World-famous enterprise Japanese fuji, sensitive materials productions such as Kodak, use enterprise select for use this low metal ion adamantane products to make raw material exactly.As seen, this product has very great function for the functional material industrial expansion.
The object of the present invention is to provide a kind of method of production high purity electronic grade adamantane products,, can produce electronic-grade high purity adamantane products by the tetrahydro-dicyclopentadiene isoversion by using the self-control composite catalyst.
Three, summary of the invention
The invention provides a kind of method of producing electronic grade adamantane products, form by the reaction of tetrahydro-dicyclopentadiene isoversion; With the self-control composite catalyst is Primary Catalysts, and its consumption is 5～50% of a tetrahydro-dicyclopentadiene weight, and optimum amount is 5～25% of a tetrahydro-dicyclopentadiene weight; Temperature of reaction is 30～180 ℃, is good with 30～100 ℃, and reaction pressure is a normal pressure; It is characterized in that: be solvent with the halohydrocarbon, consumption is 5～50% of a tetrahydro-dicyclopentadiene weight, and optimum amount is 15～25% of a tetrahydro-dicyclopentadiene weight.
Description of drawings:
Accompanying drawing is a technological process block-diagram of the present invention.
Four, embodiment
Existing combined process flow diagram is described below producing electronic grade adamantane products technology:
In the dried and clean reactor, add tetrahydro-dicyclopentadiene, ethylene dichloride and catalyzer, be warming up to 80 ℃ and carried out isomerization reaction 2 hours; Extract at the adding solvent oil then, reclaim catalyst recirculation and use; Extraction liquid is distilled the solvent oil recycling use; The concentrated solution crystallisation by cooling, the oven dry of centrifugal back promptly gets electronic grade adamantane.Purity 〉=99.9% by analysis, the residual total amount≤20ppm of metal ion.
Claims (4)
1. a method of producing electronic grade adamantane products is formed by tetrahydro-dicyclopentadiene (being called for short endo) isoversion reaction; With the self-control composite catalyst is Primary Catalysts, and its consumption is 5～50% of a tetrahydro-dicyclopentadiene weight; Temperature of reaction is 30～180 ℃, and reaction pressure is a normal pressure; It is characterized in that: be solvent with the halohydrocarbon, consumption is 5～50% of a tetrahydro-dicyclopentadiene weight.
2. by the method for the described production electronic grade adamantane products of claim 1, it is characterized in that: with the self-control composite catalyst is Primary Catalysts, and its consumption is 5～50% of a tetrahydro-dicyclopentadiene weight.
3. by the method for claim 1 or 2 described production electronic grade adamantane products, it is characterized in that: be solvent with the halohydrocarbon, consumption is 5～50% of a tetrahydro-dicyclopentadiene weight.
4. by the method for claim 1 or 2 described production electronic grade adamantane products, it is characterized in that: temperature of reaction is 30～180 ℃, and reaction pressure is a normal pressure.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2009100584346A CN101497550A (en) | 2009-02-26 | 2009-02-26 | Method for producing electronic grade adamantane products |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2009100584346A CN101497550A (en) | 2009-02-26 | 2009-02-26 | Method for producing electronic grade adamantane products |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101497550A true CN101497550A (en) | 2009-08-05 |
Family
ID=40944848
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2009100584346A Pending CN101497550A (en) | 2009-02-26 | 2009-02-26 | Method for producing electronic grade adamantane products |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101497550A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105175206A (en) * | 2015-10-20 | 2015-12-23 | 山东玉皇化工有限公司 | Process of preparing adamantane from C5 dicyclopentadiene |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1340483A (en) * | 2000-08-30 | 2002-03-20 | 中国科学院大连化学物理研究所 | Process for catalytically synthesizing adamantane with high output rate |
-
2009
- 2009-02-26 CN CNA2009100584346A patent/CN101497550A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1340483A (en) * | 2000-08-30 | 2002-03-20 | 中国科学院大连化学物理研究所 | Process for catalytically synthesizing adamantane with high output rate |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105175206A (en) * | 2015-10-20 | 2015-12-23 | 山东玉皇化工有限公司 | Process of preparing adamantane from C5 dicyclopentadiene |
| CN105175206B (en) * | 2015-10-20 | 2017-09-29 | 山东玉皇盛世化工股份有限公司 | A kind of technique by light dydrocarbon dicyclopentadiene adamantane |
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Application publication date: 20090805 |
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Addressee: Luo Xinping Document name: Notification of Passing Examination on Formalities |
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Owner name: YIBIN KAISITE PHARMACEUTICAL CHEMICAL CO., LTD. Free format text: FORMER OWNER: LUZHOU WANLIAN CHEMICAL CO., LTD. Effective date: 20140306 |
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Effective date of registration: 20140306 Address after: Yangchun City of Sichuan province Yibin Industrial Park 644200 Jiangan Applicant after: YIBIN CHEMIST PHARMACHEM CO., LTD. Address before: 646000 hundred towns, Luzhou, Sichuan, Luxian County Applicant before: Luzhou Wanlian Chemical Co., Ltd. |
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| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20090805 |